PL90027B1 - - Google Patents
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- PL90027B1 PL90027B1 PL1970173770A PL17377070A PL90027B1 PL 90027 B1 PL90027 B1 PL 90027B1 PL 1970173770 A PL1970173770 A PL 1970173770A PL 17377070 A PL17377070 A PL 17377070A PL 90027 B1 PL90027 B1 PL 90027B1
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/13—Amines
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/13—Amines
- A61K31/135—Amines having aromatic rings, e.g. ketamine, nortriptyline
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/275—Nitriles; Isonitriles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P25/00—Drugs for disorders of the nervous system
- A61P25/02—Drugs for disorders of the nervous system for peripheral neuropathies
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P9/00—Drugs for disorders of the cardiovascular system
- A61P9/06—Antiarrhythmics
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P9/00—Drugs for disorders of the cardiovascular system
- A61P9/08—Vasodilators for multiple indications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P9/00—Drugs for disorders of the cardiovascular system
- A61P9/10—Drugs for disorders of the cardiovascular system for treating ischaemic or atherosclerotic diseases, e.g. antianginal drugs, coronary vasodilators, drugs for myocardial infarction, retinopathy, cerebrovascula insufficiency, renal arteriosclerosis
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P9/00—Drugs for disorders of the cardiovascular system
- A61P9/12—Antihypertensives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C233/00—Carboxylic acid amides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C255/00—Carboxylic acid nitriles
- C07C255/49—Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
- C07C255/53—Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing cyano groups and hydroxy groups bound to the carbon skeleton
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/55—Design of synthesis routes, e.g. reducing the use of auxiliary or protecting groups
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- Vascular Medicine (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Nitrogen And Oxygen As The Only Ring Hetero Atoms (AREA)
- Hydrogenated Pyridines (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Description
Przedmiotem wynalazku jest sposób wytwarzania nowych racemicznych lub optycznie czynnych 1-feno- ksy-2-hydroksy-3-cykloalkiloaminopropanów i ich soli addycyjnych z kwasami.Nowym zwiazkom odpowiada wzór 1, w którym R oznacza grupe alkilowa, zawierajaca do 5 atomów wegla, Ri oznacza grupe nitrylowa (-C^N), lub chlorowiec, R2 oznacza wodór, chlorowiec, grupe nitrylowa lub grupe alkilowa, alkoksylowa lub alkenylowa, zawierajaca do 5 atomów wegla, R3 oznacza wodór, chlorowiec, grupe alkilowa lub alkoksylowa, zawierajaca do 5 atomów wegla i n oznacza liczbe calkowita 2-7.Nowe zwiazki wytwarza sie wedlug wynalazku, przez dwuazowanie zwiazku o wzorze 2, w którym R, R2 i R3 i n maja wyzej podane znaczenie i ogrzewanie z cyjankiem miedziawym wzglednie z halogenkiem miedzia- wym.Zwiazki o wzorze 2 zawieraja juz gotowy szkielet 1-fenoksy-2-hydroksy-3-cykloalkiloaminopropanu i'mozna je wytwarzac wychodzac z odpowiedniego fenolu, który poddaje sie reakcji z epichlorohydryna i utworzony 1-fenoksy-2,3-epoksypropan wprowadza w reakcje z cykloalkiloamina.Zwiazki otrzymywane sposobem wedlug wynalazku posiadaja asymetryczny atom wegla w grupie CHOH i wskutek tego wystepuja jako racematy i w postaci optycznych antypodów. Te ostatnie mozna otrzymac przez rozdzielenie racematu za pomoca zwykle uzywanych kwasów pomocniczych, takich jak kwas dwubenzoilo-D^ • winowy lub kwas D-3-bromokamforo-8-sulfonowy, jak równiez przez stosowanie optycznie czynnych zwiazków wyjsciowych.Otrzymywane sposobem wedlug wynalazku 1-fenoksy-3-cykloaminopropanole o wzorze 1 mozna w znany sposób przeprowadzic w fizjologicznie dopuszczalne sole addycyjne z kwasami. Odpowiednimi kwasami sa: kwas solny, kwas bromowodorowy, kwas siarkowy, kwas metanosulfonowy, kwas maleinowy, kwas octowy, kwas szczawiowy, kwas mlekowy, kwas winowy lub 8-chloroteofilina.Zwiazki o wzorze 1 wzglednie ich fizjologicznie dopuszczalne sole addycyjne z kwasami wykazuja w badaniach na swinkach morskich, jako zwierzetach doswiadczalnych, wartosciowe wlasciwosci terapeutyczne, w szczególnosci dzialanie 0-adrenolityczne i mozna je wskutek tego stosowac do leczenia i profilaktyki schorzen naczyn wiencowych serca i arytmii serca, zwlaszcza tachycardii, w medycynie. Równiez dzialanie obnizajace2 90027 cisnienie krwi jest pod wzgledem terapeutycznym interesujace.Szczególnie wartosciowymi sa przy tym takie zwiazki o wzorze 1, w którym R oznacza grupe metylowa, R3 i R3 oznaczaja zwlaszcza wodór, a równiez grupe alkilowa i Rt oznacza przede wszystkim grupe nitrylowa (w szczególnosci w polozeniu 2 lancucha propanolowego) i n ¦ 4, 5 lub 6. Równiez, gdy R oznacza grupe metylowa, Ri oznacza chlorowiec, a R2 oznacza wodór, lub grupe metylowa, a R3 oznacza wodór, a n ¦ 4,5 lub 6 zwiazki wykazuja silne dzialanie 0-adrenoJityczne. Szczególnie wartosciowymi pod wzgledem terapeutycznym sa: 1-(2-nitrylofenoksy)-2-hydroksy-3-(1-metylocyklopentylo)-aminopropan oraz 1-(2-nitrylofenoksy)-2-hydro- ksy-3-(1-metylocykloheksylo)-aminopropan, 1-(2-chloro-5-metylofenoksy)-2-hydroksy-3-(1-metylocyklopenty*- lo)-aminopropan i 1-(2-bromofenoksy)-2-hydroksy-3-(1-metylocykloheptylo)-aminopropan wzglednie Ich fizjolo¬ gicznie dopuszczalne lole addycyjna z kwitami, 1-(2-nltrylofanokiy)-2-hydrokiy-3-(1-metylocykloptntylo)-imlno- \-propan Jest izczagólnle Interesujacym wskutek twego znacznego dzialania mtagonlttyczntgo wobec Izoprotere- nolu, przy prawie calkowitym brak wlasnego dzialania powodujacego rzadkoskurcz. Szczególnie aktywnymi sa zwiazki, które w grupie fenylowej sa podstawione grupa nitrylowa w polozeniu 2 i równoczesnie nizsza grupa alkilowa, zwlaszcza metylowa w polozeniu 5, np. 1-(2-nitrylo-5-metylofenoksyy-2-hydroksy-3-(1-metylocyklop- entyloamino)-propan, 1-(2-nitrvlo-5-metvlofenoksy)2-hydroksy-3-(1-metylocykloheksyloamino)-propan i 1-(2-nt* trylo-5-metylofenoksy)-2-hydroksy-3-(1-metylocykloheptyloamino)-propan, wzglednie fizjologicznie dopuszcza¬ lne sole addycyjne tych zwiazków z kwasami.Dawka jednostkowa zwiazków otrzymywanych sposobem wedlug wynalazku wynosi 1—300 mg, zwlaszcza —100 mg (doustnie) lub 1—20 mg (pozajelitowo).Galenowa obróbke zwiazków otrzymywanych sposobem wedlug wynalazku do zwykle uzywanych form uzytkowych, takich jak roztwory, emulsje, tabletki, drazetki lub preparaty o przedluzonym dzialaniu, przepro¬ wadza sie w znany sposób, stosujac zwykle galenowe srodki pomocnicze, nosniki, srodki rozkruszajace, wiazace' lub poslizgowe, substancje smakowe, slodzace, srodki do powodowania przedluznego dzialania i ulatwiajace- rozpuszczanie.Otrzymywane sposobem wedlug wynalazku zwiazki mozna laczyc z innymi substancjami o dzialaniu farmakodynamicznym, takimi, jak np. srodki rozszerzajace naczynia wiencowe, sympatikomimetyczne, glikozydy nasercowe lub srodki uspokajajace.Przyklad I. Chlorowodorek 1-(2-cyjanofenoksy)-2-hydroksy-3-(1-metylocykloheksyloamino)-prcpanu.Do goracego roztworu z 5 g siarczanu miedzi, 5,8 g cyjanku miedzi i 30 ml wody powoli wkrapla sie roztwór soli dwuazoniowej, wytworzonej z 3,52 g (0,01 mola) chlorowodorku 1-(2-aminofenoksy)-2-hydroksy-3- (l-metylocykloheksyloamino)-propanu, 4 ml stezonego HCI, 20 ml wody i wodnego roztworu 1,4 g (0,01 mola) NaN02. Po 30 minutach mieszania w temperaturze 90°C oziebia sie ialkalizuje za pomoca NaOH. Po dodaniu chloroformu oddziela sie nierozpuszczalne czesci. Faze organiczna wyodrebnia sie, przemywa woda i suszy nad MgS04. Po oddestylowaniu CHCI3 pozostalosc rozpuszcza sie w etanolu i dodaje eterowy roztwór HCI.Wytracajace sie krysztaly przekrystalizowuje sie jeszcze raz w etanolu dodajac eter. Wydajnosc: 950 mg.Temperaturatopnienia: 161—164°C.Przyklad II. Chlorowodorek 1-(2-nJtrylofenoksy)-2-hydroksy-3-(1-metylocykloheksyloamino)-proparW, * 3,52 g (0,01 mola) chlorowodorku 1-(2-aminofenoksy)-2-hydroksy-3-(1-metylocykloheksyloamino)-pro- cpanu rozpuszcza sie w 20 ml H20 i 4 ml stezonego HCI. 1,4 g (0,02 mola) NaN02 rozpuszcza sie w 5 ml wody i powoli wkrapla sie do roztworu aminy. Przez chlodzenie lodem utrzymuje sie temperature 0° do +5°C. Po zakonczeniu dodawania utrzymuje sie roztwór jeszcze przez 15 minut w temperaturze okolo 0°C. 5g CuS04 x 5H20 (0,02 mola), 5,8 g KCN (0,04 mola) i 30 ml H2 O laczy sie i mieszajac ogrzewa do 90°C.Roztwór dwuazoniowy miesza sie z goracym roztworem Cu/I/CN i calosc utrzymuje sie przez 30 minut w temperaturze 90°C. Po oziebieniu i zadaniu 10% roztworem NaOH ekstrahuje sie chloroformem. Roztwór CHCI3 przemywa sie woda, suszy nad MgS04 i zateza. Pozostalosc rozpuszcza sie w etanolu i zakwasza alkoholowym roztworem HCI. Po dodaniu eteru produkt wykrystalizowuje. Po jeszcze jednym przekrystalizo- waniu z ukladu alkohol/eter otrzymuje sie 950 mg produktu, o temperaturze topnienia: 161—163°C.Przyklad III. Chlorowodorek 1-(2-nitrylo-5-metylofenoksy)-2-hydroksy-3-(1-metylocykloheksyloam- ino)- propanu. 2,92 g (0,01 mola) 1-(2-amino-5-metylofenoksy)-2-hydroksy-3-(1-metylocykloheksyloamino)-propanu roz¬ puszcza sie w 20 ml wody i 6 ml stezonego HCI. 1,4 g (0,02 mola) NaN02 rozpuszcza sie w 5 ml wody i powoli wkrapla podczas mieszania do roztworu aminy. Przez oziebianie lodem utrzymuje sie temperature 0° do +5°C.Po zakonczeniu dodawania roztwór utrzymuje sie przez 15 minut w temperaturze okolo 0°C. g CuS04 X 5H20 (0,02 mola), 5,8 g KCN (0,09 mola) i 30 ml H2 O laczy sie i podczas mieszania ogrzewa90027 3 do temperatury 90°C. Roztwór dwuazoniowy wkrapla sie podczas mieszania do goracego roztworu Cu/I/CN i pozostawia przez 30 minut w temperaturze 90°C do przereagowania. Po oziebieniu i zadaniu 10% NaOH ekstrahuje sie chloroformem. Ekstrakt chloroformowy przemywa sie woda, suszy nad MgS04 izateza.Pozostalosc rozpuszcza sie wacetonitrylu i zakwasza alkoholowym roztworem HCI. Wykrystalizowany chloro¬ wodorek przekrystalizowuje sie jeszcze raz z acetonitrylu. Temperatura topnienia: 170-173°C, wydajnosc: 500 mg.Analogicznie, jak w wyzej podanych przykladach, wytwarza sie nastepujace zwiazki o wzorze 1: Temperaturatopnienia Temperaturatopnienia Rt R, Rf R n °C (chlorowodorek) 2-Br 2-a 2-Br 2-Br 2-a 2-a 2<:n ^CN 2-a 2-CN 2-CN 2-CN 2-CN 2-CN H "CsH, H II -CHj -CH, H H -CH, H 4-a -CH, -ch, H H H H H H H H H H H H H H H CH, CH, CH, CH, CH, C2H5 C,H5 i-C,H7 CH, CH, CH, CH, CH, CH, 4 4 6 6 6 6 4 4 156-157 170-172 157-158 167-168 174-177 179-180 157-158 200-201 191-194 160-161 194-196 192-194 143-146 132-134 ^ 2 II R WZ0R 1 ^73^0CH2-CH0H-CH2-NH-CjCH2)n WZ0R2 Prac. Poligraf. UP PRL naklad 120+18 Cena 10 zl PL PL PL PL PL PLThe subject of the invention is a process for the preparation of new racemic or optically active 1-phenoxy-2-hydroxy-3-cycloalkylaminopropanes and their acid addition salts. The new compounds correspond to formula 1, in which R is an alkyl group containing up to 5 carbon atoms, Ri is nitrile (-C1N), or halogen, R2 is hydrogen, halogen, nitrile or an alkyl, alkoxy or alkenyl group of up to 5 carbon atoms, R3 is hydrogen, halogen, alkyl or alkoxy of up to 5 atoms carbon and n is an integer of 2-7. The new compounds are prepared according to the invention by diazotizing a compound of formula 2, wherein R, R2 and R3 and n are as defined above, and heating with cuprous cyanide or with a cuprous halide. 2 already contain the ready skeleton of 1-phenoxy-2-hydroxy-3-cycloalkylaminopropane and can be prepared starting from the corresponding phenol, which is reacted with epichlorohydrin and formed 1-phenoxy-2,3 -epoxypropane is reacted with cycloalkylamine. The compounds according to the invention have an asymmetric carbon atom in the CHOH group and therefore occur as racemates and in the form of optical antipodes. The latter can be obtained by resolving the racemate with the usual auxiliary acids, such as dibenzoyl-D 4 -tartaric acid or D-3-bromocamphor-8-sulfonic acid, as well as by using optically active starting compounds. The phenoxy-3-cycloaminopropanols of the formula I can be converted into physiologically acceptable acid addition salts in a known manner. Suitable acids are: hydrochloric acid, hydrobromic acid, sulfuric acid, methanesulfonic acid, maleic acid, acetic acid, oxalic acid, lactic acid, tartaric acid or 8-chlorothophyllin. Compounds of formula I or their physiologically acceptable acid addition salts show in tests in guinea pigs, as experimental animals, valuable therapeutic properties, in particular o-blocking activity, and can therefore be used for the treatment and prevention of coronary artery diseases and cardiac arrhythmias, especially tachycardia, in medicine. The blood pressure lowering effect2 90027 is also therapeutically interesting, especially the compounds of formula I in which R is methyl, R3 and R3 are especially hydrogen, and the alkyl group and Rt are primarily the nitrile group (in especially in the 2-position of the propanol chain) and n 4, 5 or 6. Also, when R is methyl, Ri is halogen and R2 is hydrogen or methyl and R3 is hydrogen, and n ¦ 4,5 or 6 the compounds show strong 0-adrenaline action. Therapeutically valuable are: 1- (2-nitrilophenoxy) -2-hydroxy-3- (1-methylcyclopentyl) -aminopropane and 1- (2-nitrilephenoxy) -2-hydroxy-3- (1-methylcyclohexyl) -aminopropane, 1- (2-chloro-5-methylphenoxy) -2-hydroxy-3- (1-methylcyclopenty * yl) -aminopropane and 1- (2-bromophenoxy) -2-hydroxy-3- (1-methylcycloheptyl) ) -aminopropane or their physiologically acceptable flower additive, 1- (2-nltrilophanokiy) -2-hydroxyy-3- (1-methylcyclopentyl) -imyl-1-propane is especially interesting due to its considerable mtagglottic action against isoprotective compounds. nole, with almost complete absence of its own bradycardia effect. Particularly active are compounds which in the phenyl group are substituted with a nitrile group in position 2 and, at the same time, with a lower alkyl group, especially methyl in position 5, e.g. 1- (2-nitrile-5-methylphenoxy-2-hydroxy-3- (1- methylcyclopentylamino) propane, 1- (2-nitril-5-methylphenoxy) 2-hydroxy-3- (1-methylcyclohexylamino) propane and 1- (2-nt * tryl-5-methylphenoxy) -2-hydroxy- 3- (1-methylcycloheptylamino) -propane, relatively physiologically acceptable acid addition salts of these compounds with acids. The unit dose of the compounds according to the invention is 1-300 mg, especially 100 mg (orally) or 1-20 mg (parenterally). The galenic treatment of the compounds according to the invention into the usual use forms, such as solutions, emulsions, tablets, dragees or long-acting preparations, is carried out in a known manner, usually using galenic auxiliaries, carriers, disintegrants, binders. or lubricants, flavors, sweeteners, sro Prolonging and dissolving agents. The compounds obtained according to the invention can be combined with other substances having a pharmacodynamic effect, such as e.g. coronary vasodilators, sympathomimetic agents, cardiac glycosides or sedatives. Example 1- 2. -cyanophenoxy) -2-hydroxy-3- (1-methylcyclohexylamino) -prcpan. To a hot solution of 5 g of copper sulphate, 5.8 g of copper cyanide and 30 ml of water is slowly added dropwise the solution of the diazonium salt prepared from 3.52 g (0.01 mol) 1- (2-aminophenoxy) -2-hydroxy-3- (1-methylcyclohexylamino) propane hydrochloride, 4 ml concentrated HCl, 20 ml water and an aqueous solution of 1.4 g (0.01 mol) NaN02. After 30 minutes of stirring at 90 ° C, it is cooled and made alkaline with NaOH. When chloroform is added, the insoluble matter is separated. The organic phase is separated, washed with water and dried over MgSO 4. After CHCl 3 has been distilled off, the residue is dissolved in ethanol and ethereal HCl is added. The crystallizing crystals are recrystallized once more in ethanol while adding ether. Yield: 950 mg. Melting point: 161-164 ° C. Example II. 1- (2-N-ethylphenoxy) -2-hydroxy-3- (1-methylcyclohexylamino) -proparW hydrochloride, * 3.52 g (0.01 mol) 1- (2-aminophenoxy) -2-hydroxy-3- ( 1-methylcyclohexylamino) propane is dissolved in 20 ml of H 2 O and 4 ml of concentrated HCl. 1.4 g (0.02 mol) of NaNO 2 are dissolved in 5 ml of water and slowly added dropwise to the amine solution. The temperature is kept at 0 ° to + 5 ° C by cooling with ice. After the addition is complete, the solution is kept for an additional 15 minutes at a temperature of approximately 0 ° C. 5 g of CuSO 4 x 5H 2 O (0.02 mol), 5.8 g of KCN (0.04 mol) and 30 ml of H 2 O are combined and heated to 90 ° C with stirring. The diazonium solution is mixed with the hot Cu / I / CN solution and The whole thing is kept for 30 minutes at a temperature of 90 ° C. After cooling and treating with 10% NaOH solution, extraction was carried out with chloroform. The CHCl3 solution is washed with water, dried over MgSO4 and concentrated. The residue is dissolved in ethanol and acidified with an alcoholic HCl solution. Upon addition of ether, the product crystallizes out. After a further recrystallization from the alcohol / ether system, 950 mg of product are obtained, mp: 161-163 ° C. Example III. 1- (2-Nitrile-5-methylphenoxy) -2-hydroxy-3- (1-methylcyclohexylamino) propane hydrochloride. 2.92 g (0.01 mol) of 1- (2-amino-5-methylphenoxy) -2-hydroxy-3- (1-methylcyclohexylamino) propane were dissolved in 20 ml of water and 6 ml of concentrated HCl. 1.4 g (0.02 mol) of NaNO 2 are dissolved in 5 ml of water and slowly added dropwise with stirring to the amine solution. The temperature is kept at 0 ° to + 5 ° C by cooling with ice. After the addition is complete, the solution is kept at a temperature of about 0 ° C for 15 minutes. g of CuSO 4 X 5 H 2 O (0.02 mol), 5.8 g of KCN (0.09 mol) and 30 ml of H 2 O are combined and, with stirring, heated to 90 ° C. The diazonium solution is added dropwise to the hot Cu / I / CN solution with stirring and left to react for 30 minutes at 90 ° C. After cooling and quenching with 10% NaOH, extraction was carried out with chloroform. The chloroform extract is washed with water, dried over MgSO 4 and dried. The remainder is dissolved in acetonitrile and acidified with an alcoholic HCl solution. The hydrochloride that crystallizes out is recrystallized once more from acetonitrile. Melting point: 170-173 ° C, yield: 500 mg By analogy to the examples above, the following compounds of formula 1 are prepared: Melting point Melting point Rt R, Rf R n ° C (hydrochloride) 2-Br 2-a 2 -Br 2-Br 2-a 2-a 2?: N ^ CN 2-a 2-CN 2-CN 2-CN 2-CN 2-CN H "CsH, H II -CHj -CH, HH -CH, H 4-a -CH, -ch, HHHHHHHHHHHHHHH CH, CH, CH, CH, CH, C2H5 C, H5 iC, H7 CH, CH, CH, CH, CH, CH, 4 4 6 6 6 6 4 4 156- 157 170-172 157-158 167-168 174-177 179-180 157-158 200-201 191-194 160-161 194-196 192-194 143-146 132-134 ^ 2 II R WZ0R 1 ^ 73 ^ 0CH2 -CH0H-CH2-NH-CjCH2) n WZ0R2 Printing UP PRL Edition 120 + 18 Price PLN 10 PL PL PL PL PL PL
Claims (2)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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DE1937477A DE1937477C3 (en) | 1969-07-23 | 1969-07-23 | I-phenoxy-2-hydroxy-3- (l -methylcycloalkylamino) propane, process for their preparation and medicaments containing them |
Publications (1)
Publication Number | Publication Date |
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PL90027B1 true PL90027B1 (en) | 1976-12-31 |
Family
ID=5740681
Family Applications (9)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PL1970173769A PL90028B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173765A PL90039B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173772A PL90025B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173767A PL90030B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173766A PL90038B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173770A PL90027B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970142196A PL79772B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173771A PL90026B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173768A PL90029B1 (en) | 1969-07-23 | 1970-07-21 |
Family Applications Before (5)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PL1970173769A PL90028B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173765A PL90039B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173772A PL90025B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173767A PL90030B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173766A PL90038B1 (en) | 1969-07-23 | 1970-07-21 |
Family Applications After (3)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PL1970142196A PL79772B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173771A PL90026B1 (en) | 1969-07-23 | 1970-07-21 | |
PL1970173768A PL90029B1 (en) | 1969-07-23 | 1970-07-21 |
Country Status (17)
Country | Link |
---|---|
US (1) | US3755413A (en) |
JP (5) | JPS5133106B1 (en) |
AT (9) | AT304475B (en) |
BE (1) | BE753774A (en) |
BG (9) | BG17508A3 (en) |
CH (10) | CH536813A (en) |
CS (9) | CS170528B2 (en) |
DE (1) | DE1937477C3 (en) |
DK (1) | DK140281B (en) |
ES (8) | ES382014A1 (en) |
FR (1) | FR2059551B1 (en) |
GB (1) | GB1314896A (en) |
NL (1) | NL169874C (en) |
PL (9) | PL90028B1 (en) |
RO (9) | RO60112A (en) |
SE (1) | SE370391B (en) |
YU (5) | YU34395B (en) |
Families Citing this family (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3937706A (en) * | 1969-07-23 | 1976-02-10 | Boehringer Ingelheim Gmbh | 1-(2'ethynyl-phenoxy)-2-hydroxy-3-(cycloalkyl-amino)-propanes and salts thereof |
US4021576A (en) * | 1969-07-23 | 1977-05-03 | Boehringer Ingelheim Gmbh | Pharmaceutical compositions containing a 1-(2'-ethynyl-phenoxy)-2-hydroxy-3-(cycloalkyl-amino)-propane and method of use |
US4120978A (en) * | 1970-01-08 | 1978-10-17 | Ciba-Geigy Corporation | Pharmaceutical composition for inhibiting and blocking cardioselective beta-receptors |
US4038313A (en) * | 1970-01-08 | 1977-07-26 | Ciba-Geigy Corporation | Cycloalkylureido phenoxy propanolamines |
SE354851B (en) * | 1970-02-18 | 1973-03-26 | Haessle Ab | |
US4145442A (en) * | 1972-04-04 | 1979-03-20 | Aktiebolaget Hassle | Phenoxy-hydroxypropylamines, their preparation, and method and pharmaceutical preparations for treating cardiovascular diseases |
US4038414A (en) * | 1972-06-08 | 1977-07-26 | Ciba-Geigy Corporation | Amines and processes for their manufacture |
US4035420A (en) * | 1972-07-06 | 1977-07-12 | Aktiebolaget Hassle | Substituted ureido alkylene phenoxy propanolamines |
DE2309887C2 (en) * | 1973-02-28 | 1983-11-10 | C.H. Boehringer Sohn, 6507 Ingelheim | 1-aryloxy-2-hydroxy-3-alkynylaminopropane derivatives and their physiologically acceptable acid addition salts, pharmaceutical preparations and manufacturing processes for the compounds |
US4220659A (en) * | 1974-02-22 | 1980-09-02 | Boehringer Ingelheim Gmbh | 1-Phenoxy-2-hydroxy-3-alkynylamino-propanes and salts thereof |
SE7510153L (en) * | 1974-09-12 | 1976-05-07 | American Cyanamid Co | ALKANOLAMINES |
US4165384A (en) * | 1974-11-01 | 1979-08-21 | Aktiebolaget Hassle | Amide substituted phenoxy propanol amines |
US4387103A (en) * | 1980-11-28 | 1983-06-07 | American Hospital Supply Corporation | Method for treatment or prophylaxis of cardiac disorders |
US4471127A (en) * | 1981-09-08 | 1984-09-11 | Ciba-Geigy Corporation | 1-5-Bis-(1,4-benzodioxin-2-yl)-3-azapentane-1,5-diols |
US5039801A (en) * | 1985-12-20 | 1991-08-13 | The United States Of America As Represented By The Department Of Health & Human Services | Thermal fragmentation of methylbenzylurea disastereomers or secondary amines and preparation of optically active secondary amines |
JPS6364630U (en) * | 1986-10-17 | 1988-04-28 |
-
1969
- 1969-07-23 DE DE1937477A patent/DE1937477C3/en not_active Expired
-
1970
- 1970-03-22 BG BG017138A patent/BG17508A3/en unknown
- 1970-03-23 BG BG017134A patent/BG17750A3/en unknown
- 1970-07-16 CH CH224873A patent/CH536813A/en not_active IP Right Cessation
- 1970-07-16 CH CH224373A patent/CH570363A5/xx not_active IP Right Cessation
- 1970-07-16 CH CH224973A patent/CH550139A/en not_active IP Right Cessation
- 1970-07-16 CH CH1106675A patent/CH575376A5/xx not_active IP Right Cessation
- 1970-07-16 CH CH1087370A patent/CH537360A/en not_active IP Right Cessation
- 1970-07-16 CH CH224573A patent/CH536810A/en not_active IP Right Cessation
- 1970-07-16 CH CH224473A patent/CH550140A/en not_active IP Right Cessation
- 1970-07-16 CH CH224773A patent/CH536812A/en not_active IP Right Cessation
- 1970-07-16 CH CH224273A patent/CH536809A/en not_active IP Right Cessation
- 1970-07-16 CH CH224673A patent/CH536811A/en not_active IP Right Cessation
- 1970-07-20 RO RO69799A patent/RO60112A/ro unknown
- 1970-07-20 RO RO69803A patent/RO59159A/ro unknown
- 1970-07-20 RO RO69805A patent/RO59210A/ro unknown
- 1970-07-20 RO RO69806A patent/RO59211A/ro unknown
- 1970-07-20 RO RO69804A patent/RO59209A/ro unknown
- 1970-07-20 RO RO69801A patent/RO59112A/ro unknown
- 1970-07-20 RO RO63988A patent/RO56318A/ro unknown
- 1970-07-20 RO RO69798A patent/RO60111A/ro unknown
- 1970-07-20 RO RO69802A patent/RO59089A/ro unknown
- 1970-07-21 CS CS4505A patent/CS170528B2/cs unknown
- 1970-07-21 PL PL1970173769A patent/PL90028B1/pl unknown
- 1970-07-21 PL PL1970173765A patent/PL90039B1/pl unknown
- 1970-07-21 PL PL1970173772A patent/PL90025B1/pl unknown
- 1970-07-21 CS CS4504A patent/CS170527B2/cs unknown
- 1970-07-21 CS CS4507A patent/CS170530B2/cs unknown
- 1970-07-21 GB GB3535970A patent/GB1314896A/en not_active Expired
- 1970-07-21 CS CS4503A patent/CS170526B2/cs unknown
- 1970-07-21 CS CS4508A patent/CS170531B2/cs unknown
- 1970-07-21 PL PL1970173767A patent/PL90030B1/pl unknown
- 1970-07-21 PL PL1970173766A patent/PL90038B1/pl unknown
- 1970-07-21 PL PL1970173770A patent/PL90027B1/pl unknown
- 1970-07-21 ES ES382014A patent/ES382014A1/en not_active Expired
- 1970-07-21 CS CS4506A patent/CS170529B2/cs unknown
- 1970-07-21 PL PL1970142196A patent/PL79772B1/pl unknown
- 1970-07-21 CS CS5136A patent/CS170524B2/cs unknown
- 1970-07-21 PL PL1970173771A patent/PL90026B1/pl unknown
- 1970-07-21 PL PL1970173768A patent/PL90029B1/pl unknown
- 1970-07-21 CS CS4502A patent/CS170525B2/cs unknown
- 1970-07-21 CS CS4509A patent/CS170532B2/cs unknown
- 1970-07-22 BG BG015254A patent/BG17749A3/en unknown
- 1970-07-22 BE BE753774D patent/BE753774A/en not_active IP Right Cessation
- 1970-07-22 BG BG017136A patent/BG17507A3/en unknown
- 1970-07-22 BG BG017135A patent/BG17751A3/en unknown
- 1970-07-22 US US00057353A patent/US3755413A/en not_active Expired - Lifetime
- 1970-07-22 DK DK380170AA patent/DK140281B/en unknown
- 1970-07-22 BG BG017137A patent/BG18852A3/en not_active Expired
- 1970-07-22 YU YU1860/70A patent/YU34395B/en unknown
- 1970-07-22 JP JP45063634A patent/JPS5133106B1/ja active Pending
- 1970-07-22 BG BG018645A patent/BG19132A3/en unknown
- 1970-07-23 AT AT118272A patent/AT304475B/en active
- 1970-07-23 AT AT118372A patent/AT304476B/en not_active IP Right Cessation
- 1970-07-23 AT AT118572A patent/AT304478B/en active
- 1970-07-23 AT AT117972A patent/AT306702B/en not_active IP Right Cessation
- 1970-07-23 FR FR7027291A patent/FR2059551B1/fr not_active Expired
- 1970-07-23 AT AT674870A patent/AT303706B/en not_active IP Right Cessation
- 1970-07-23 AT AT118172A patent/AT304474B/en active
- 1970-07-23 SE SE7010200A patent/SE370391B/xx unknown
- 1970-07-23 AT AT118472A patent/AT304477B/en not_active IP Right Cessation
- 1970-07-23 AT AT118072A patent/AT306703B/en not_active IP Right Cessation
- 1970-07-23 NL NLAANVRAGE7010928,A patent/NL169874C/en not_active IP Right Cessation
- 1970-07-23 AT AT118672A patent/AT306704B/en not_active IP Right Cessation
- 1970-07-24 BG BG017132A patent/BG17505A3/en unknown
- 1970-07-24 BG BG017133A patent/BG17506A3/en unknown
-
1971
- 1971-09-09 ES ES394917A patent/ES394917A1/en not_active Expired
- 1971-09-09 ES ES394914A patent/ES394914A1/en not_active Expired
- 1971-09-09 ES ES394916A patent/ES394916A1/en not_active Expired
- 1971-09-09 ES ES394913A patent/ES394913A1/en not_active Expired
- 1971-09-09 ES ES394919A patent/ES394919A1/en not_active Expired
- 1971-09-09 ES ES394918A patent/ES394918A1/en not_active Expired
- 1971-09-09 ES ES394915A patent/ES394915A1/en not_active Expired
-
1973
- 1973-06-06 JP JP48063730A patent/JPS5210863B1/ja active Pending
- 1973-06-06 JP JP48063728A patent/JPS5210861B1/ja active Pending
- 1973-06-06 JP JP48063727A patent/JPS5238556B1/ja active Pending
- 1973-06-06 JP JP48063729A patent/JPS5210862B1/ja active Pending
-
1975
- 1975-10-07 YU YU2544/75A patent/YU34396B/en unknown
- 1975-10-07 YU YU2545/75A patent/YU34662B/en unknown
- 1975-10-07 YU YU2546/75A patent/YU34663B/en unknown
- 1975-10-07 YU YU2551/75A patent/YU34113B/en unknown
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