SU941377A1 - Process for producing di-(2,3-isopropylidene glyceryl) phosphite - Google Patents

Description

This invention relates to the chemistry of phosphorus compounds, in particular, to an improved process for the preparation of DI- (2,3-isopropylideneglyceryl) phosphite of the formula

CH2-5H- (H20

II

about

vCrfT dH,

which can be used in the chemical and pharmaceutical industry,

The closest in technical essence and achievable results: The proposed method is a method of obtaining di- (2.3 isopropylideneglyceride) phosphyte by reacting hexaethyltriamidophosphite with isopropylideneglycerol at a molar ratio of reagents equal to 1: 2, followed by treatment of the forming diethyl dimethylamine with 3

α-zopropyl; -1 denglycerol) phosphorous acid with glacial acetic acid in benzene at. The yield of the target product 53 per hexa ethyl triamide phosphite l.

The disadvantage of this method is the relatively low yield of the target product.

The purpose of the invention is to increase the yield of the target product.

The goal is achieved by the fact that according to the method of obtaining

Claims (1)

15 (March 2 izopropilidenglitseril) phosphite geksaegiltriamidofosfit general formula is reacted with an equimolar amount izopropilidenglitserina at 110-130 C and obrazuyu20 schiys tetraetildiamid 2,3-izopropilidonglitserilfosforistoy acid sequentially treated with acetic anhydride and at izopropilidenglitserinom. 39 The proposed method allows to reduce the yield of di- (2,3-isopropylide benglyceryl) phosphite to} %%. Example. Preparation of di- (2,3-isopropylideneglyceryl) phosphite. 12.35 g of phosphoric acid hexaethyl triamide and 6.6 g of isopropylideneglycerol are heated at 110 ° -30 ° until the liberated diethylamine is stopped. The remaining reaction mass is kept under vacuum to remove residues of low-boiling products and is distilled. 12.8 (83it) tetraethyl diamide 2,3 isopropylidene glyceryl phosphorous acid is obtained. T, kip. 52-55C / 0.2 mmHg. To 12.8 g of tetraethyl diamide 2,3-isopropylideneglyceryl phosphorous acid, with stirring, add 5, 1 g of acetic anhydride at such a rate that the temperature of the reaction mass does not exceed 30, stirred at this temperature of 30 minutes and, according to the same conditions, add 6.6 g of isopropylidene glycerol are added, the mixture is stirred at 30–35 ° C for 1 h, acetic acid diethylamide is removed in vacuo, the residue is distilled. 12.1 g (93) of Di-C2.3 isopropylideneglyceryl) phosphite are obtained, b.p. 89 90 ° C / 0.02 mmHg,, it564, dflj857. MR-p Found 71.12. Calculated 70.8. 4 The yield of di- (2,3-isopropylideneglyceryl) phosphite per hexa ethyl triamide of phosphorous acid is 77.6%. The invention of the method for producing di- (2,3-isopropylideneglyceryl) phosphite of the formula (H2- (H- (1H20 "N./0 CH2 THj by reacting hexaethyltriamidophosphite with isopropylideneglycerol at an elevated temperature, about the fact that with the aim of to increase the yield of the target product, the initial reagents are used in an equimolar ratio, the process is carried out at 110-130 ° C and the resulting isomethyl tetraethyl diamide 2,3 isopropylidene glyceryl phosphorous acid is successively treated with acetic anhydride and isopropylideneglycerol at 10-35 ° C. tion, the received note in the examination 1. Predvoditelev DA Chubar TG, E.E Nifant'ev, New approach to creating diglitserofosfatnyh, tionfosfatnyh and phosphonate structures. ZHOH, 1976, 6, 291 (prototype).