SU133865A1 - The method of obtaining di- (K-W-carboxyhexyl-beta-aminoethyl) -ether vinylphosphonic acid - Google Patents

Description

A method is proposed for the preparation of vinylphosphonic acid di- (M- (o-carboxyhexyl-p-aminoethyl) ester), which is the monomer for the synthesis of high-molecular-weight phosphorus-containing compounds.

The essence of the proposed method lies in the fact that w-amino-enanthic acid acts on di- (p-chloroethyl) ester of vinylphosphonic acid and produces di- (H-O-carboxyhexyl-p-aminoethyl) ester of vinylphosphonic acid, from which sodium alkoxide is isolated are vinylphosphonic acid di (N- (o-carboxyhexyl-p-aminoethylbol) ether).

The reaction proceeds as follows:

 (OCH2CH2C1) 2 + 2NH2 (CH,) in UNC -

O2C, H5ONa

, CH2MN (CH2) bCOOH 2 - 2HC1 O - OCH2CH2NH (CH2) 6COOH 2

Example. In a three-necked flask equipped with a reflux condenser, a thermometer and a dropping funnel, place a solution of 11.65 g (0.05 mol) of vinylphosphinic acid di- (p-chloroethyl ether) vinylphosphinic acid in 50 ml of 80% aqueous alcohol and pour the solution 14 into it. , 5 g

No. 133865 2 -

(0.1 mol) (O-amino-enanthic acid in 50 ml of 80% aqueous alcohol. The mixture is heated on a water bath with constant stirring for 4 hours. After the completion of the reaction, the solvent is distilled off and 26.25 g of residue are obtained Dihydrochloride di- (Mm-carboxyhexyl-p-aminoethyl) ester of vinylphosphonic acid in the form of a glassy mass of yellow color. (The yield is close to quantitative).

Di (L-oucarboxyhexyl-p-aminoethyl) vinylphosphonate dichlorohydrate is taken up in an alcoholic solution of sodium alkoxide (2, & g of sodium in 100 ml of abs. Alcohol). The solution is separated from the precipitated salt, the alcohol is distilled off, and the residue is vinylphosphonic acid di (M-co-carboxyhexyl-p-aminoethyl) ester. So pl.-70 ° (Yield 80% of theoretical).

Found in%:, 3; 93

Mol weight 434 (according to potency. titration)

Calculated in%:, 88; , 2.

Mol weight 450.

Subject invention

The method for preparing di- (N-w-carboxylhexyl-p-aminoethyl) vinylphosphonic acid ester, otlichyuyushh; vinylphosphinic acid chloroethyl ester and di- (K-o; carboxyhexyl-p-aminoethyl) vinylphosphinic acid dichlorohydrate are obtained; vinylphosphinic acid dichlorohydrate from which sodium dihydrogen phosphine ester is selected as sodium alcoholate;