SU488824A1 - Method for preparing -2-chloropropylene (0,0-dialkyl dithiophosphoryl) dialkyl thiophosphates - Google Patents

Description

the presence of acid or alkaline catalysts.

However, it is not possible to obtain non-metric esters using these methods; but. Generally, two residues of different 0.0 dialkyl A. nitrophosphoric acids or a residue C, O - dialkylthio and a residue 0.0 - diapki.pditio {humoric acids.

A known method for producing bis-dithiofs ™ sphats involves the addition of 0,0-dialkyl dithiophosphoric acids to their S-allyl esters in the presence of iti-. 1 chaters of free radical reazhggy.

The novel compounds of the indicated general formula contain as a 0.0-dialkyl digiophosphoripacin and 0.0-dialkylthiophosphorus groups connected by a 2-chloropropene bridge. The combination of the dithio- and thiophosphoric acids and the chlorine atom in the A-position of the scientific research institute to the phosphoryl parts of the molecule in the molecules of these compounds should be related to their biological activity.

The method of obtaining S; S 2-chorpropile 5 (O. O-dialkyldithiophosphoryl) dialkylthio-phosphates is based on a known reaction with an compound of organophosphorus sulfenyl shorks to unsaturated compounds that have not previously been applied to unsaturated phosphorus acids.

According to the proposed method, 0,0-dialkyl allyldithiophosphate general formula

(EOLPSCH,

Z

where fi is alkyl,

subjected to interaction with 0, O-dial.hylphosphoryl sulfenyl chlorohydride of the total formula

(R 0) jPSW,

about

where ft is alkyl.

The process is carried out in an organic solvent medium, for example, benzene. Temgeratla reaction is desirable to support. Target products excrete kg. local receptions.

As indicated by chromatographic analysis, the reaction of the practical one;: if it is not accompanied by the formation of side products, the yield of the target products is quantitative. For technical purposes, the resulting compounds can be used non-prod. after removing the solvent from the reaction mixture without further purification.

Example 1. - 2-chloropropylene (o, 0 - DNETH-datiophosphoryl) -dietz-1-thiophosphate.

2.26 g (0.01 mol) of 0-diethyl S-allyldithiophosphate is dissolved in 10 M; I benzene, 2.04 g (0.01 mol) of 0.0-diethyl phosphoryl sulphenyl chloride is added to the solution while stirring. The mixture was allowed to stand at room temperature for 5 hours. After distilling off the solvent, it is distilled in vacuum at 115 ° C / 10 mmHg.

Art.

gf

3.9 g (91%) of substance are obtained, d.

Claims (2)

1.2608, 1.5220 (for a crude, non-distilled product H-1.5204), JVJK D found 104.25; calculated 104.97. Found,%; R 14.08; 14.22; 322.14; 22.26; Ct 7.84; 8.06. C HjiOsPaSja., Calculated,%: R 14.37; S 22.32; CIS, 22. Example 2. S, S 2 -chloropropi.len- (o, O-- DIPROPYLDDITIOPHOSPHORIL DIET 1LTIO phosphate. 2.54 g (o, 01 mol) of 0.0-dipropyl-S-alkyl dithiophosphate is dissolved in 10 ml of benzene, and 2.04 g (o, 01 mol) of 0.0-di ethylphosphoryl sulfenyl chloride g-1 is added to the solution with stirring . The mixture is left for 5 hours at room temperature: e. Ate; -; distilling off the solvent, the reaction product was distilled under vacuum at 120 ° C / / 10 mm Hg. Art. Ryogvanpogs ggolukuta And-1.51 Oe) ,, ,, .. - „„ В -...,. D 20.36; 20.68; C1 С;, гН.О, Р „З.С1  r at. -., LZ, 49; Calculated,%: P , 72, Thing (LO), P -SCH. SNCH, 5-P (OL),. - it- 2 ) SSGO where R and R is alkyl, characterized in that 0,0 - ЦИШЛК.ИЛ- S -allildithio rosphate of formula (.H-m, S where R is alkyl, is reacted with 0,0-dialkylphosphoryl sulphenylchloride form.: s.1b (), PSC, 41 ABOUT where R. is alkyl, in the medium of an organic solvent, followed by separation of the target product by known techniques. 2. The method according to claim 1, about tl and h and y - y and so that the process is carried out at 10-30 ° C.