SU166693A1 - - Google Patents

Description

Nitrochloroalkylphosphiates of the type NOa-R-P (x) -2, where x is alkoxy, halo or

I II C1 O

amide group, and R is alkyl, not described in the literature.

The proposed method is that the alkenyl phosphinate is reacted with nitrile chloride at a low temperature.

The process is carried out at a temperature of from-10 to -5 ° C. The reaction mass is stirred for 5-6 hours, the nitrile chloride is passed, at room temperature, after which it is subjected to distillation and the reaction product is separated at 104-106 ° C / 1 J1. The yield of products is 40-65%.

The compounds obtained are light yellow liquids that are stable during storage. Their structure is proved by the data of physical and elementary analyzes.

Synthesis of iitrochloride alkyl phosphinates can be used as a pesticide to intermediates for the synthesis of organo-organic compounds, in particular, as starting materials for the preparation of nitroalkenyl phosphinates, which can be used as monomers for polymerization.

In a four-necked flask with a capacity of 50 ml, equipped with a stirrer and a reflux condenser with a calcium chloride tube, a thermometer and a bubbler, 0.1 mol of 0.0-diethylviiyl phosphinate is placed and, with vigorous stirring, 0.12 mol of nitrile chloride is passed in, maintaining the temperature of the reaction mass from -10 to -5 ° C. Then stirring is continued at room temperature for 5-6 hours, after which the reaction mass is transferred to a Claisen flask and subjected to distillation, the reaction product is taken at 104-106 C / 1 mm. Exit 41.5o / o.

0,0-diztil-hloritiroethylphosphinate - light yellow liquid with a faint odor, stable under snoring; d 1.2612; p 1.4570; LHO 52.66; MRo calculated 51.80.

Found,%: C - 30.38, 30.36; H - 5.96, 6.06; P-13.24, 13.30; N - 4.97, 5.07; C1-1222, 15.28. CoHisPOsNCl.

Calculated,%: C - 29.28; P - 5.32; P - 12.62; N - 5.69; C1 - 14.46.

Note 2.

When carrying out a similar process with 0.1 mol of 0,0-di- {p-chloroethyl) -viiyl phosphinate and 0, 2 mol of nitrile chloride obtained 0.0 - di - (p-chloroethyl) - chloronitroethyl phosphinate - thick, light yellow, non-distilled liquid with a faint odorless odor, stable at snoring; yield 67.4%; df 1,5246; n2 ° 1.4992; , 61; Mrc

calculated 61.54.

C - 24.00, 23.95; H Found,%:

 3.98, 3.96; P- 10.96, 10.80; N 3.42, 3.66; CI - 31.80, 31.83.

Calculated%

C - 22.92; H - 3.53; P - 9.87; N 4.46; C1 - 33.69.

Example 3

In a similar process with 0.1 mol of 0,0-diethylallylphosphinate and OL2 mol of nitrile chloride, 0.0-diethylchloronitropropylphosphinate-thick, light yellow, non-distilled liquid with a weak uncharacteristic pickup was obtained, and was stable; yield 65.4%; df 1.2805; , 4660; MR D 56.24; MR D calculated 56.42.

Found, "/ o. C - 33.28, 33.20; H - 5.03, 5.24: P-12.16, 12.69; N - 4.68, 4.73; C1-14.07, 13.72. CTHisPOsNCl.

Calculated,%: C -32.31; H - 5.82; P - 11.92; N - 5.38; C1-13,68.

Subject invention

1. A method of producing nitrochloroalkylphosphinates of the general formula NOo-R - P (l :),

Claims (2)

I I C1 o where l: is an alkoxyl, halo, or amide group, and R is alkyl, characterized in that the alkenyl phosphinate is reacted with nitrile chloride at a reduced temperature. 2. The method according to claim 1, characterized in that the process is carried out at a temperature of from -10 to -5 ° C.