SU410020A1 - - Google Patents

Description

one

This invention relates to a process for the preparation of heterocyclic phosphorus derivatives, namely, novel (polyfluoro) alkyleidiox- diclotriphosphazenes, which can be used as monomers for the organofluorine polymer monomers with cyclophosphazene units.

A known method for producing 1,3,5-tris (polyfluoro) alkylenedioxycyclotrnphosphazenes by reacting hexachlorocyclotriphosphazene with 3 mol (polyfluoro) alkylene glycol

in the presence of a tertiary amine in an organic solvent medium. The resulting compounds are polymerized to form three-dimensional structures.

New (polyfluoro) alkylenedioxncyclotrnphosphazenes containing only one cyclic organofluorine ester group are capable of forming linear polymers.

A method is proposed for the preparation of (nolfluoro) alkylenedioxycyclotrnphosphazenes of the general formula

1: 1 ratio in the presence of a hydrogen chloride acceptor, such as triethylamine, in an organic solvent medium, such as diglyme, dioxane, followed by treatment of the resulting 1,1- (iolifluoro) alkylenedioxytetrachlorocyclotriphosphazene with alkali metal fluoro-alcoholate and isolation of the target product using known techniques.

The process is preferably carried out by heating.

Example 1. In a 500 ml flask, a solution of 32.8 g (0.094 mol) of hexachlorocyclotriphosphazene and 20 g (0.094 mol) of hexafluoroimylene glycol in 250 ml of diglyme was poured and 9.5 g (0.094 mol) of triethylamine in 50 ml of diglyme were added to it. The reaction mixture is heated at 80-90 ° C for 5 hours, then another 9.5 g (0.094 mol) of triethylamine is added in 50 ml of diglyme and the mixture is heated for 6 hours. The product is filtered off and the precipitate is washed with 100 ml of absolute diethyl ether. The solvent is evaporated in vacuo. The residue is 1,1-hexafluoroimylenedioxy - 3,3,5,5 - tetrachlorocyclo triphosphazep, m.p. 52-54 ° C, t. Kip. 90 ° C / 4-10 mm Hg. Art.

Found,%: C 12.16; And 0.90; C1 28.65; F 23.70; N 8.50; R 18.95.

CsMiFgCLiNsPaOa.

Calculated,%: C 12.32; P 0.82; C1 29.16; F 23.40; 8.62; P 19.10.

In the P1K spectrum of the compound, there is no visible iolos1. in the region of 3180-3200, it is characteristic for OH-gruiy (polyfluoro) alcohols. The spectrum shows that soydeppe has a siiro structure.

The residue is dissolved in 100 ml of d, ethyl ether and while cooling with ice, 122.0 g (0.55 mol) of sodium heptafluorobutnlate in 400 ml of ether are added dropwise over 40 minutes. The reaction mixture is heated to the boiling point of ether, the ether is refluxed and the boil is further heated at 130-150 ° C for 5 hours. The reaction product is treated with water, with a 10% solution of hydrochloric acid and again with water, then dried over and heated in vacuo. Select the fraction with so c. 155-160 ° C / 3 mm Hg Art. 54.75 g of 1,1-hexafluoro-imideide 3, 3,5,5-tetrabis - (heptafluorobutoxy) - cyclotriphosphazene, 1.3415 1.7259 are obtained. Yield 51% (based on hexachlorocyclo triphosphazeu).

Found,%: C 21.80; H 0.91; F 57.1; N 3.82; R 7.85.

G2iHi2F34N3P306.

Calculated,%: C 22.09; H 1.05; F 56.62; N 3.68; R 8.15.

Subject invention

Claims (2)

1. A method for producing (solifluoro) alkyl-idlyccyclotriphosphaseae of the general formula JCF) h. sn sn Chr / - N N it . j / h% OCH2Rf N Rf is polyfluoroalkyl; where m is an integer characterized in that the hexachlorocyclophosphazene is reacted with (iolifluoro) alkylene glycol in the presence of an accelerator of hydrogen chloride in an organic solvent medium, followed by treatment with a 1: 1 1,1- (iolifluoro) alkylenedioxytetracyclophosphazene fluorine alcohol of an alkaline metal and the target product by the alkaline metal and the target product. 2. A method according to claim I, characterized in that the process is carried out with heating.