SU569287A3 - Method of preparation of benzhydryloxyalkylamine derivatives or salts thereof - Google Patents

Description

(54) METHOD OF OBTAINING BENZHYDRET BENZHYDRYLOXYLKYLAMINE

OR THEIR SALTS 35 of the compound of formula II. Target products are recovered in the form of a plug or tail. The process is preferably carried out at 80 ° C with the use of sodium amide as the base and benzene as solvent. Salts are preferably prepared without isolation of compounds of the formula I by reaction with a pharmaceutically acceptable inorganic or organic acid. Example. To a mixture of 4.2 g of sodium amide and 80 ml of dry benzene was added 27.9 g (0.12 mol) of cv - methyl - p - chlorbeishydryl and then 17.6 g (0.1 mol) of N - (3 chloroethyl) heptamethylenimine. Mix the mixture for 20 hours at its boiling temperature. Then the mixture is cooled and washed twice, (20 ml each) with water and 4 times (50 ml each) 2 n. hydrochloric acid. The acidic extracts are combined and the pH of this combined acidic extract is adjusted to pH 9 by the addition of a concentrated aqueous solution of NaOH. Collect the organic layers obtained by extraction (3X30 ml) with benzene. The solvent is distilled off and the residue is purified by distillation. By this way, N - 2 - (p - chloro - a - methyl - o: - feshbenzyloxy) - ethyl - heptamethylenimine boils at 58-162 ° C at a pressure of 0.005 mm Hg; 55% yield; p 1.5574. The hydrofumar salt of this compound, after recrystallizing from lanolum, has a so on. 144-145C. 6%; C 66.31; H7.03; C17.26; N2.86. Iadeno,%: C, 66.36; H 7.18; C1 7.35; N 2.78. EXAMPLE 2 To a mixture of 4.2 g of sodium amide and 80 ml of dry benzene, 27.9 g (0.12 mol) of a-methyl and chlorobenzhydrol and 16.2 g (0.1 mol) are successively added. N - ((3-chloroethyl) -hexamethylenia. The mixture is stirred for 20 hours at the boil and then cooled and rinsed 2 times (20 ml each time) with water. The solution is dried over Mg2S04 to complete distance of water and then treated with charcoal. HC1-gas. The crystallized product which has been obtained is filtered through a glass filter and then recrystallized from acetone to give N-2 - (a - methyl chloro - a - phenylbene zyloxy) - ethyl hexamevode 65%, type 1min min of hydrochloride with a mp of 170-17 ° C, calculated as%: C 67.12; H 7.41 C1 18.07; N 4.06. Found:% C67.03; H7.47; C1 17.95; N4.12. Examples 3-11. Using the method variations described in examples 1-2, the compounds described in the table are prepared Table.

Claims (3)

Claims 1. A method for producing benzogadryloxyalkylamine derivatives of the general formula CH3 X- (((U,)) where X is a halogen atom, methyl or methoxy group — together with the nitrogen atom to which it is bound, forms a heterocyclic core that can to be condensed with a benzene core and may be substituted by one and two w methoxy groups, n is an integer equal to 2, 3 or 4, or their salts, characterized in that the cyclic imine derivative of the general formula 11 / QM- (CH2) nY where A and p have the indicated meanings, Y is a halogen atom, odvergayut interaction with benzgidrolnym derivative of general formulas C HL-OH S 56928 4 where X has the indicated values, in organ-4. way on either. 1-3, characterized in It is known that it is a process that is carried out at at 60-1.20 C at O-Siy / r.-HOM excess of the compound Formula II, with the following selection of targeted sources of information taken into account products in V11de of the base of Igi salt. 5 during exernysis: 2. Method of clause 1, on tl and h a r y with the fact that 1. Weigand-Hilgetag. Experimental methods include sodium amide. Organic chemistry, M., Chem. 1968, p. 33.S. 3. Method according to nil. 1 and 2, different 2. Patent of Great Britain No. 942152, cl. C 2 C in that benzene is used as the solvent. 1963.