SU407915A1 - - Google Patents

Description

METHOD OF OBTAINING ORGANOPHOSPHORUS COMPOUNDS

one

This invention relates to a process for the preparation of novel organophosphorus compounds of the general formula

(RO), P - CH, - CH - R

II

OR - P - OR

II Oh

where R is alkyl;

R is alkoxycarbonyl;

R is alkyl or CH2COOAlk.

These compounds can be used as extractants of rare metals.

The method of producing organophosphorus compounds of the above general formula is based on the Arbuzov reaction, which was not previously used to synthesize compounds of a similar structure.

According to the method, the derivatives of a, p-diphosphorus-substituted carboxylic acids of the general formula

(RO), P-CH, -CH-R P (OR). where R is alkyl; R is alkoxycarbonyl, is reacted with halide al-30

halides or esters of halocarboxylic acids of the general formula where alkyl or CHjCOOAlk;

X is halogen.

Target products are recovered by known techniques.

All reactions are carried out in a stream of dry argon.

Example 1. Preparation of a (O-ethylmethylphosphinato) -p- (O, O-diethylphosphonato) -propionic acid ethyl ester.

To 14 g (0.04 mol) of a- (O, 0-diethylphosphonite) -p- (O, O-diethylphosphonato) ethyl ester ethyl ester ethyl acetate is added dropwise while cooling (15 ° C) and stirring 5.7 g (0 , 04 mole) methyl iodide. Then the reaction mixture is heated in a water bath in an appliance with a downward cooler and a receiver. Ethyl iodide is distilled off. After cessation of the release of ethyl iodide, the reaction mixture is distilled in vacuo. Obtain 11 g (80% of theoretical) (EtO), PCHj - CH - COOEt III О CH, -POEt T. KIP. 143 ° C / 0.05 mm, df 1Д562; po 4490 Mnvpide 79,89; IKBvych 80,34. Found,%: C 41.75; H 7.66; R 17.95. CiaHseOrPs Calculated,%: C 41.85; H 7.61; P 17.99. IR spectrum V with. Example 2. Obtaining ethyl ester of wasp (0-ethylcarbethoxymethylphosphinato) - p- (O, O diethylphosphonato) propionic acid. To 12 g (0.044 mol) (EtO), PCH, CHCOOEt II I O P (OEt), add 5 g (0.046 mol) of chloroacetic acid methyl ester. At the same time observe a slight warming (). Then the reaction mixture is heated for 3.5 hours at 100 ° C. After distillation of the reaction mixture in vacuo, 12 g (67% of the theoretical) (EtO) sPCH, -CH-COOEt (About MeOOC-CH, -P-OEt J 20., 20 145 ° C / 0.01 mm) are obtained. ; d4 1.1741; According to T. bil. 1.4445. MKvnaid 91.09; MKpvych 91.39. Found,%: C 41.65; H 7.53; R 15.79. Ci4H28O9P2 Calculated,%: C 41.85; H 7.03; R 15.40. IR spectrum V 0 0 1740; v 1735. Subject of the invention. A method for the preparation of organophosphorus compounds of a common forms (RO), P — CH, —CH — R II where R is alkyl; R-alkoxycarbonyl; R-alkyl or CHaCOOAlk, differing from the fact that the derivatives of a, riphosphate-substituted carboxylic acids are both formula (RO), P-CH, -CH-R or P (OR), de R and R have the above values, They are reacted with halogenated alkyls or halidecarboxylic esters with subsequent isolation of the target product by known methods.