SU449063A1 - Method for producing alkylene (arylene) bismonoalkylphosphonites with higher alkyl radicals - Google Patents

Description

This invention relates to a process for the preparation of organophosphorus compounds, namely, new alkylene (arylene) bismonoalkylphosphonites with higher alkyl radicals of the general formula KO ..- OR P-A-P, O where R is higher alkyl; A is alkylene or arylene. These compounds can be used as intermediates in the synthesis of phosphorus organic compounds, including polymeric materials. The proposed method for the preparation of compounds of general formula I is that alkylene (arylene) bisdichlorophosph of the general formula A — PCl, C1, P with higher alcohol and the selection of the target product is known)) methods. Alkylep (arylene) bisdichlorophosphine, lower alcohol and higher decrease are preferably taken in a molar ratio of 1: 2, respectively. The process in the second stage is preferably carried out in the presence of kata / shzator, for example, mineral acids. Dip off the lower alcohol and water, it is advisable to remove it by azeotropic distillation at 12 O2 ° C with an organic solvent, for example, with xylene. The reaction proceeds quantitatively. Example. 1,2-Ethylene Bismonohexylphosphonite. o, 2 mol of anhydrous methanol is added over a period of 5 to 10 minutes O, O5 mol 1, 1,2-ethylene bisdichlorophosphine; at the same time, the reaction mass boils. Then to the mixture

34

0.25 mol of hexanol is poured in and the reaction is: Calculated,%: C 51.55; H 9.90;

The mass is boiled in a Dean-Stark apparatus; p 18.99; Mr 86 34.

until the termination of the distillation of water (6-8 Excess alcohol is distilled off in vacuum and the VIC spectrum, (240 O), P-O

the remainder receive the target product, (1250)

h 1.468, d 1.0473. Output-1OO% .o

ilD 4 Under the same conditions, they get a drudan,%: C 51.2; H 9.84; P 18,42. Good compounds, properties and data analysis

Atfjjj 86.66; which are listed in the table.

4 19О63 Subject of the invention 1. Method of producing alkylene {ariden bismonoalkylphosphonites with higher alkyl radicals of the general formula P-A-PC, c / L o where R is higher alkyl; A is alkylene or arylene, which is an alkyl (arylene) bisdichlorophosphine of the general formula - A - PC where A is alkylene or arylene, I interact with a lower alcohol followed by heating the reaction mass with a higher alcohol and the selection of the target product known techniques. 2. Method pop. 1, characterized in that alkylene (arylene} bis-dichlorophosphine, lower alcohol and higher I alcohol is used in a molar ratio respectively, 3. The method according to PD is different and methanol is used as the lower alcohol. 4. Method according to Claim 1, characterized in that the heating is carried out under conditions of azeotropic distillation of water and lower alcohol at 120-2OO ° C, preferably in the presence of an organic solvent, for example xylene. h and s - 111 and so that the second stage of the reaction is carried out in the presence of catalysts, for example a miner lnr 1x acids.