SU504778A1 - Method for producing monoalkyl phosphites - Google Patents

Description

(54) METHOD FOR MAKING MONO-ALKYLPHOSPHITES

one

The invention relates to the field of production of phosphorous acid, in particular to a new method of obtaining monoalkyl phosphites of the general formula:

"",. L

where R is alkyl.

Monoalkyl phosphonates are of great interest as intermediates for the synthesis of various, including new, types of phosphorus-gapic compounds.

Monoalkyl phosphite production pruning procedures are known, based on the dialkyl phosphite hydrolysis of dialkyl phosphite reaction with phosphorous acid. These methods require the preliminary synthesis of dnalkyl phosphites.

Monoalkanol phosphites are also obtained by the interaction of phosphorous acid with alcohols by boiling the reaction mixture in a solvent. The reaction does not always proceed unambiguously and usually dialkylphosphites are formed along with monoalklphosphites.

Often used is a method for the preparation of myoalkyl phosphonates, based on the hydrolysis of a.m. chemical derivatives and chlorophosphites. Disadvantage of this

The method requires the use of a hydrogen chloride acceptor and the associated difficulty in isolating the final product.

In order to simplify the process, a new method for the preparation of monoalkyl phosphites is proposed. It consists in the fact that the product — the interaction of phosphorus trichloride and tert-butanol at a molar ratio of 1: 2 — is reacted with alcohols.

The process is preferably carried out in an organic solvent, for example tert.-butyl chloride, at a temperature of from 20 to 60 ° C.

The product of the interaction of phosphorus trichloride and tert-butanol is obtained by adding the calculated quality of the tertiary alcohol to phosphorus trichloride with vigorous stirring and a temperature of 20-60 ° C in an organic solvent, preferably at the boiling point of the reaction mass. After separation of the main mass of hydrogen chloride, the calculated amount of the corresponding alcohol is added to the product of the reaction, also at a temperature of 20-60 ° C. The reaction is usually verified under these conditions in 30-60 minutes. After removal of the volatile nobiches products, preferably vacuuming, the residue is obtained, nj a-Kticheski with kol 1 natural output, products

... .. 3

n a form of colorless transparent ipcrczype blueiicH liquid.

An example. Obtaining monodecyl phosphate.

A solution of 0.3 g-mol of tert-butyl in 10 ml of tert-butyl chloride is added over 15 to 20 minutes to a solution of 0.15 g / mol of 3 h of chlorine phosphorus in 15 ml of tert-butyl chloride. However, due to the exothermic reaction, a weak boiling of the reaction mass is maintained. After mixing the reagents, the mixture is boiled, continuing stirring, for 30–60 minutes, while the bulk of the hydrogen chloride formed in the reaction (0.12–0.13 g-mol) is removed from the mixture. Then to the reaction mass was added 0.15 gmol I-decyl alcohol at such a rate that the mixture boiled slightly (due to the exothermic reaction). After dissolving the first monoal kil phosphites

Claims (2)

1. The method of producing moioalkylphosphites based on trivalent phosphorus chlorides, is distinguished by the fact that, in order to simplify the process, the product of the interaction of phosphorus trichloride and tert-butanol Initially, the Sediment (PV) mixture was boiled until the B1 division of hydrogen chloride was stopped, evacuated at 20–60 ° C (100–20 mm) to constant weight, catching tert-butyl chloride in a cooled lui. The residue is obtained as a colorless transparent liquid. Yield -100%, 1.4270, df 1.1280, MRo 31.44, calculated 31.94. Found,%: C 34.71; H 8.48; R 22,21. ScNPOZR. Calculated,%: C 34.80; H 8.04; R 22.50. Acid equivalent of 130.7; calculated 138.1. A similar result is obtained when carrying out the reaction in an environment of methylene chloride. Similarly, with the yield of -100%, other compounds are obtained, the list of which and the analysis data are shown in the table. ..HE ROK H at a molar ratio of 1: 2 is subjected to reaction with alcohols. 2. A method according to claim 1, from 1 to 5 with the fact that the process is carried out in an organic solvent, for example tert.-butyl chloride, at a temperature of from 20 to 60 ° C.