SU449060A1 - Method for preparing thiocarbamoyl thiophosphonates - Google Patents

Description

one

The invention of otiosips to a new method of obtaining previously unknown comic phosphorus compounds of a common forgule

C1-A-0OR

/

RS-P-NHC-S-P-R

11 o

S and

| de A - alkylene;

R is alkyl, aryl;

C - aralkyl, aryl;

about

H is alkyl,

which have pesticidal activity and can be used as fungicides, defoliants, desiccants and other

physiologically active substances, as well as intermediates for the synthesis of new organic phosphorus compounds.

The interaction of isocyanates with organophosphorus compounds containing mobile dt of phosphorus is known. However, O-chloralkyl - 3 .organothiophosphoric acid isocyanates were not previously introduced into this reaction.

A method is proposed for the preparation of thiocarbamone thiophosphonates by the interaction of O-chloroalkyl-S-organothiophosphoric acid isothiocyanates with thiophosphonic acid O-alkyl esters, followed by isolation of the desired product by known methods.

The process proceeds according to the scheme; where A, R, I and R are as defined above. The reaction proceeds under mild conditions better when heated to 45-5 ° C and an equimolar ratio of the initial reagents in an inert organic solvent. Target products are formed quantitatively. They are sedentary painted id bones. The degree of their purity and structure was confirmed by elementary and spectral analyzes, as well as by using paper and column chromatography. I PRI me R, O-Butyl - S - N (O - - chloroethyl - S - butylthiophosphoryl) - tricarbamoylphenylthiophosphonate To a solution of O, O2 mol O-butylphenylthiophosphonic acid in benzene with stirring and 20-25 ° С benzene solution is added O, O2 mol of isothiocyanate O- 0 - chloroethyl - $ - butylthiophosphoric acid The reaction mass is stirred for 1 hour at room temperature, 3 hours at 45-5 ° C, and the solvent is distilled off under reduced pressure. The product is obtained as a brownish oily liquid, 20 i cxion, .54JO, d 1,256O, quantitative. Found,%: N2.81; P 12.44; 818.71. C.H gClNO P Sg. Calculated,%: N 2.78; P 12.30; S 19.05. In the IR spectrum of the obtained compound, the following characteristic absorption regions () were detected: 545 and 565 (P - S - C), 670 (C – C1), 880 (P - N), 1040 (P – O – C), 1140 ( С SS), 1260 (), 1445 (Р-aryl), 1470 (СН СН - def.), 288О-2980 (- shaft), 3400 (Н –И-shaft). Compounds are obtained in a similar way, the list and data of the analysis of the l groups are presented in the table.

Subject invention

The method of obtaining thiocarbamoylthio (} yusphonates, characterized in that the isothiocyanates of O-chloralkyl-g-yrganothiophosphoric 1 $ islothed to mutually interfere with the O-alkyl esters of thiophosphonic acids in an inert environment

 organic solvent followed by isolation of the target product are known

I tricks.