SU371240A1 - METHOD OF OBTAINING SALTS O, O-DI- (AMINOPHENYL) - dithiophosphoric acids - Google Patents

Description

one

The present invention relates to the field of preparation of dithiophosphoric acid derivatives, namely, to a method for producing new salts of 0,0-di- (amynophenyl) - dithiophosphoric acids of the general formula

.TSM

 II

- V-0 S

where M is a salt-forming cation.

These compounds can be used for the preparation of phosphorus-containing dyes, analytical reagents, physiologically active substances.

A method of producing dithiophosphoric acid diesters is known by reacting phosphorus pentasulfide with alcohols or phenols, in the latter case in the presence of organic bases. However, attempts to obtain O, O-di- (aminophenyl) -dithiophosphates from phosphorus pentasulfide and aminophenols in the presence of organic bases or without them were unsuccessful. This forms a mixture of products that cannot be separated. Obviously, aminophenols react with

phosphorus pentasulfide is not only hydroxyl, but also, like aniline, on the amino group.

In order to obtain new salts of O, O-di (aminophenyl) -dithiophosphoric acids containing amino groups in benzene cores, a method has been proposed based on a previously unknown reaction of the transesterification of tetratiophosphonic acid diesters.

According to the proposed method, salts of dialkyltetratiophosphoric acids of the general formula

(RS), PSM, II S

where R is alkyl,

M - salt-forming cation.

subjected to interaction with aminophenols.

The process is carried out with heating in an inert organic solvent, preferably in benzene or toluene, while boiling

the reaction mixture.

As salts of DNA alkyltetraophosphoric acids, it is desirable to use salts of amines, the best of all is triethylammonic. These salts are stable and have greater solubility in organic solvents than

sodium or potassium, which significantly reduces the heating time of the initial components and contributes to an increase in the yield of the product.

The starting salts are prepared from mercaptan, phosphorus pentasulfide, and triethylamine with a reagent ratio of 4: 1: 2.

Target products are isolated by known techniques. The mercaptan released as a result of the substitution reaction can be regenerated and returned to obtain the starting salts of dialkyl tetratiophosphoric acids.

Example. The triethylammonium salt of O, Od- (o-aliphenyl) -dithiophosphoric acid.

0.01 gm mol of the tributylamine salt of dibutyl tetratiophosphoric acid and 0.02 g mol of o-aminophenol are boiled in 15 liters of toluene for 40-45 hours. The precipitate is filtered off and recrystallized from acetone. 2.7 g (66%) of the triethylammonium salt of O, 0-di (o-amyvophenyl) -dithiophosphoric acid are obtained; m.p. 112-113 ° C

Paydeno,%: P 7.51; 7.88; S 14.99; 15.16; N 9.86; 9.93.

C18H28NzO2P52.

Calculated,%: P 7.45; S 15.43; N 10.10.

Subject invention

Claims (4)

1. A process for the preparation of salts of O, O-di- (aminophen: yl) -dithiophosphoric acids, characterized in that the salts of dialkyltetraphosphoric acids are reacted by heating with aminophenols in an inert organic solvent, followed by isolation of the target product by known techniques. 2. A method according to claim 1, characterized in that triethylammonic acids are used as the salts of the dialkyl tetratiophosphoric acids. 3. Method according to paragraphs. I and 2, characterized in that benzene or toluene is used as an inert organic solution. 4. Method according to pi. 1, 2 and 3, characterized in that the process is carried out at boiling of the reaction mixture.