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SU578315A1 - Method of preparing cyclic alkylenethio phosphites - Google Patents

Method of preparing cyclic alkylenethio phosphites

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Publication number
SU578315A1
SU578315A1 SU7602368719A SU2368719A SU578315A1 SU 578315 A1 SU578315 A1 SU 578315A1 SU 7602368719 A SU7602368719 A SU 7602368719A SU 2368719 A SU2368719 A SU 2368719A SU 578315 A1 SU578315 A1 SU 578315A1
Authority
SU
USSR - Soviet Union
Prior art keywords
cyclic alkylene
alkylenethio
phosphites
thiophosphites
dialkyl
Prior art date
Application number
SU7602368719A
Other languages
Russian (ru)
Inventor
Николай Кириллович Близнюк
Римма Семеновна Клопкова
Людмила Дмитриевна Протасова
Борис Федорович Андронов
Борис Сергеевич Широков
Original Assignee
Всесоюзный научно-исследовательский институт фитопатологии
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Всесоюзный научно-исследовательский институт фитопатологии filed Critical Всесоюзный научно-исследовательский институт фитопатологии
Priority to SU7602368719A priority Critical patent/SU578315A1/en
Application granted granted Critical
Publication of SU578315A1 publication Critical patent/SU578315A1/en

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Description

А. Смесь 0,05 моль 1,3-неопентиленхлорфосфита и 0,05 моль третичного амилмеркаптана нагревают при перемешивании и температуре бани 120-130°С в течение 4 ч, вакуумируют и перегонкой остатка выдел ют продукт. Выход 89%; т. кип. 120-122°С/5-7 мм рт. ст. 154-156°С/15 мм рт. ст.A. A mixture of 0.05 mol of 1,3-neopentylene chlorophosphite and 0.05 mol of tertiary amyl mercaptan is heated with stirring and at a bath temperature of 120-130 ° C for 4 hours, evacuated and the product is distilled off. Yield 89%; m.p. 120-122 ° C / 5-7 mm Hg. Art. 154-156 ° C / 15 mmHg Art.

Вещество быстро кристаллизуетс ; т. нл. 7375°СThe substance crystallizes rapidly; so nl 7375 ° С

Найдено, %: С 35,93; Н 6,65; Р 18,20; S 18,83.Found,%: C 35.93; H 6.65; P 18.20; S 18,83.

CsHuOaPS.CsHuOaPS.

Вычислено, %: С 36,13; Н 6,69; Р 18,63; S 19,29.Calculated,%: C 36.13; H 6.69; P 18.63; S 19.29.

ИК-спектр, см-: 2350 (Р-Н), 1050-1040 (Р-О-С), 900-840 (цикл), 670 (P S).IR spectrum, cm-: 2350 (Р-Н), 1050-1040 (Р-О-С), 900-840 (cycle), 670 (P S).

ПМР-снектр: бонз акс. 0,92 м. д., бонз экв. 1,29 м. д., бсн2 3,4-4,3 м. д., бр-и 7,78 м. д., 602 ГЦ.PMR: Bonz Ac. 0.92 ppm, bonz eq. 1.29 ppm, bsn2 3.4-4.3 ppm, br-7.78 ppm, 602 HZ.

Б. Смесь 0,03 моль 1,3-неопеитилхлорфосфита , 0,03 моль третичного амилмеркаитана и 7 мл хлороформа кип т т в течение 6 ч, вакуумируют и перегонкой остатка выдел ют продукт.B. A mixture of 0.03 mol of 1,3-neo-epityl chlorophosphite, 0.03 mol of tertiary amylmercaitane and 7 ml of chloroform is boiled for 6 hours, evacuated and the product is distilled off by distillation of the residue.

Выход 76%; т. кип. 90-92°С/2-3 мм рт. ст., т. пл. 73-75°С.Yield 76%; m.p. 90-92 ° C / 2-3 mm Hg. Art., t. pl. 73-75 ° C.

Найдено, %: С 35,85; Н 6,69; Р 17,81; S 18,96.Found,%: C 35.85; H 6.69; R 17.81; S 18.96.

Пример 2. Получение 1,3-бутилентиофосфита .Example 2. Obtaining 1,3-butylenethiophosphate.

Смесь 0,05 моль 1,3-бутиленхлорфосфита и 0,052 моль третичного амилмеркантана нагревают при перемешивании и температуре 120- 130°С в течение 5 ч, вакуумируют и перегонкой остатка выдел ют продукт.A mixture of 0.05 mol of 1,3-butylene chlorophosphite and 0.052 mol of tertiary amyl mercanthan is heated under stirring at a temperature of 120-130 ° C for 5 hours, evacuated and the product is isolated by distillation of the residue.

Выход 72%, т. кип. 88-90°С/2-3 мм рт. ст., 1,5215; df 1,2402; MRn 37,38; вычислено 37,42.Yield 72%, kp. 88-90 ° C / 2-3 mm Hg. Art., 1.5215; df 1.2402; MRn 37.38; calculated 37.42.

Найдено, %: С 31,81; Н 6,06; Р 19,75; S 20,63.Found,%: C 31.81; H 6.06; R 19.75; S 20.63.

C4H902PS.C4H902PS.

Вычислено, %: С 31,57; Н 5,97; Р 20,35; S 21,07.Calculated,%: C, 31.57; H 5.97; R 20.35; S 21.07.

Пример 3. Получение 2,3-бутилеитиофосфита .Example 3. Obtaining 2,3-butylethiophosphite.

Смесь 0,05 моль 2,3-бутиленхлорфосфита и 0,052 моль третичного амилмеркаптаиа нагревают при перемешивании и температуре бани 120-130°С в течение 4 ч, вакуумируют и перегонкой остатка выдел ют продукт.A mixture of 0.05 mol of 2,3-butylene chlorophosphite and 0.052 mol of tertiary amyl mercaptaine is heated with stirring and at a bath temperature of 120-130 ° C for 4 hours, evacuated and the product is distilled off.

Выход 75%; т. кип. 82-84°С/2-3 мм рт. ст.; 1,4935; df 1,2032.75% yield; m.p. 82-84 ° C / 2-3 mm Hg. v .; 1.4935; df 1.2032.

xVlRn 36,77; вычислено 37,42. Найдено, %: С 31,66; Н 5,78; Р 19,64; S 20,78.xVlRn 36.77; calculated 37.42. Found,%: C 31.66; H 5.78; R 19.64; S 20.78.

C4H902PS.C4H902PS.

Вычислено %: С 31,57; Н 5,97; Р 20,35; S 21,07.Calculated%: C 31.57; H 5.97; R 20.35; S 21.07.

Claims (2)

1.Способ получени  циклических алкилентиофосфитов из циклических алкиленхлорфосфитов , отличающийс  тем, что, с целью повышени  выхода продукта, циклический алкилеихлорфосфит подвергают взаимодействию с третичным амилмеркаптаиом при температуре 60-130°С.1. A method of producing cyclic alkylene thiophosphites from cyclic alkylene chlorophosphites, characterized in that, in order to increase the yield of the product, cyclic alkylene chlorophosphite is reacted with a tertiary amyl mercaptaium at a temperature of 60-130 ° C. 2.Способ по п. 1, отличающийс  тем, что процесс провод т в среде органического растворител .2. A method according to claim 1, characterized in that the process is carried out in an organic solvent medium. Источники информации, прин тые во внимание при экспертизеSources of information taken into account in the examination 1.Авторское свидетельство СССР Ле 390095, кл. С 07F9/21, 1971.1. Authors certificate of USSR Le 390095, cl. From 07F9 / 21, 1971. 2.Krawiecki Cz., Michalski J. Action of Hydrogen Sulphide on Dialkyl and Diaryl Phosphorochloridites . New Synthesis of Dialkyl and Diary Thiophosphites and Tetraalkylthiopyrophosphites . JoLirn. Chem. Soc., 1960, p. 881-885.2. Krawiecki Cz., Michalski J. Action of Hydrogen Sulphide on Dialkyl and Diaryl Phosphorochloridites. New Synthesis of Dialkyl and Diary Thiophosphites and Tetraalkylthiopyrophosphites. JoLirn. Chem. Soc., 1960, p. 881-885.
SU7602368719A 1976-06-02 1976-06-02 Method of preparing cyclic alkylenethio phosphites SU578315A1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4341722A (en) * 1979-07-06 1982-07-27 Ciba-Geigy Corporation 2-Thiono-(2H) [1,3,2] dioxaphosphorinanes (phospholanes)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4341722A (en) * 1979-07-06 1982-07-27 Ciba-Geigy Corporation 2-Thiono-(2H) [1,3,2] dioxaphosphorinanes (phospholanes)

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