SU334837A1 - Process for preparing tatraalkyldiamides of beta,beta-dichlorovinylphosphoric acid - Google Patents

Abstract

1. A method for producing tetraalkyldiamidovr, n, is a chloroylphenyl phosphate-noy acid based on chloral, characterized in that, in order to simplify the process, chloral is reacted with phosphorous tetraalkyl diamide of phosphoric acid in an inert organic solvent. The POP.1 method, characterized in that the tetraalkyl-diamides of phosphorous acid are taken in excess.

Description

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: The invention relates to methods for producing phosphoric acid diamido esters. A new method for the preparation of tetraalkyldnamides (L, L) of dichlorovinyl phosphoric acid of the general formula L II is proposed. p-osn sag 2 where P and R-alkyl. These compounds have insecticidal and acaricidal effects and can be used to protect plants from pests. A known method for the preparation of tetraalkyldiamides fb, / L-dichlorophenylphosphoric acid by reacting chlorine and tetraalkyldiamidoalkyl phosphites with heating. This method allows to obtain the target products with a fairly high yield, however, the starting tetraalkyldiamidoalkyl phosphites are difficult to access and unstable compounds. They easily disproportionate, therefore the products synthesized on their basis are usually a mixture of hardly separated substances. To simplify the process, a new method for producing tetraalkyldia-30 MIDOV / 5, (5-dichlorovinyl phosphoric acid, not previously used for the synthesis of similarly constructed substances) has been proposed. According to the described method, chloral is reacted with phosphorous acid tetra-aluminum-amide, which it is desirable to take in excess. The process is carried out in an inert organic solvent j, for example diethyl ether. The desired 4Q products are isolated by known methods. Their yield reaches 56%. Example 1. Preparation of tetramethyldiamide p, p, -dih lorvinylphosphoric acid. 32.5 g of chloral in 100 ml of absolute diethyl ether is added dropwise to a solution of 60 g of tetramethyldiamide phosphorous acid in 200 ml of absolute diethyl ether. The reaction is carried out at minus with stirring. After displacing, the reaction mixture is stirred for 1 5 h at the same temperature. A precipitate of dimethylamine hydrochloride is observed. Then the precipitate is filtered off, the filtrate is dispersed. A fraction with mp of 5–87 ° C 1 mm Hg is isolated. 4800 d2 1.2573, yield 25 g (46%). Found 55.8 {calculated 54.2. R 0.6 (system-acetone: benzene 1: 1); 0.5 (chloroform-system), sorbitol-alumina P, Brockman activity. Found.%: C 28.85; H5.83; R 12.17. Calculated,%: C 29.16; And 5.30; R 12.53. Example 2. Obtaining tetraethylamine l, ft-dichlorophenylphosphoric acid. 34.5 g of chloral is added dropwise to a solution of 90 g of phosphorous tetraethyl diamide in 200 ml of absolute diethyl ether at room temperature while stirring. Diethylamine hydrochloride precipitates. After the reaction mixture has been located at room temperature for 4.5 hours, the precipitate is filtered off and the filtrate is dispersed. A fraction with m Kip is recovered. 80 85 C / 10mmHg | P 1.4762; d, 1531, yield 40 g (56%) of MRj, found 74.16; calculated 72.62. R 0.7 (system-acetone: benzene: 1) (system-chloroform), aluminum sorbitol P degree of activity according to Yerokman. Found,%: C 39.83; H 6.74, P 10.30. Calculated,%: C 39.61; H 6.98; R 10.21.

j B P T B

Claims (2)

NOAH ACID based on chloral, characterized in that, in order to simplify the process, chloral is reacted with tetraalldiamides of phosphorous acid in an inert organic solvent. 2. The method according to claim 1, characterized in that the tetraalkyl diamides of phosphorous acid are taken in excess. The invention relates to methods for producing diamide esters of phosphoric acid. A new method is proposed for producing tetraalkyl diamides β, β dichlorvinylphosphoric acid total where R and formulas R 'is alkyl. These compounds have insecticidal and acaricidal action and can be used to protect plants from pests. A known method for producing tetra-15 alkyl diamides of β, β-dichlorovinylphosphoric acid by the interaction of chloral with tetraalkyl diamidoalkylphosphites by heating. This method allows to obtain the target products with a satisfactory 20 but high yield, however, the initial tetraalkyl diamidoalkyl phosphites are difficult to access and unstable compounds. They are easily disproportionate; therefore, products synthesized on their basis are usually a mixture of hardly separable substances. To simplify the process, a new method for the preparation of tetraalkyl diamides of 30 β, β-dichlorovinylphosphoric acid, not previously used for the synthesis of similarly constructed substances, is proposed. According to the described method, chloral is reacted with tetraal-35 kyl diamides of phosphorous acid, which are preferably taken in excess.