SU453408A1 - Method of producing phenylvinylcyclosiloxanes - Google Patents

Description

one

The invention of othositei to the field of iolucine cyclic monomeric silicon organo-compounds containing several winnyl groups in the cycle.

The above mentioned organosilicon cyclic phenylinvinylsiloxanes can be used both for the synthesis of ontic and transparent network organo-cyclocarboxylic oxane polymers, and for the synthesis of neyai and branched polyorganoxy-cyclocarboxyloxanes by the reaction of hydride nolodellI1NI. 1)) Moreover, the fiilvinylcyclosiloxia obtained can be used to obtain by catalytic polymerization linear polysiloxanes with vinple groups at silicon atoms as heat-resistant additives in the preparation of various polysploxane resins.

A known method for the production of cyclonoxanes by the reaction of heterofunctional condensation of organosilicate compounds with organohispochlosplans. However, this method has not been previously used for the preparation of phenylvinpcyllosiloxanes. Describes the method for producing phenylvinlcyclosiloxapes, which consists of carrying out a heterofunctional condensate of the optics 1,3-dioxy-1,3-diphenyl 11 Bin disiloxane with fenplpnpl dichlorosilapol or a, d-dichlorophenylvinylsiloxanes in the presence of a sample, using a group of people using a group of people using a group of people who are using a group of people who are using a group of people who are using a group of people who are using a group of people who are using a group of in organic solvent according to the scheme

СГНз СеНц

Ii. Akiept HO-Si-0-Si-OH + CeH; (CH, CHiSiCl2

, lc6HsiCH, CHlSiO + nonufiep

SbNe SbH5CgHs C.HS

II I (j, l acceptance НО-51-0-81-ОН-СС1-51- (0-81 -) "С1

IIII CH CHjCH CH2, H5 () SLO Hr where, 2, 3, 4 P T. d .; ni 4, 5, 6, 7 p.

The proposed method allows to obtain various fenplplcyclosloxapes with high yields (50-66% of theoretical and possible).

Monitoring the progress of the process of obtaining fennvinylcyclosphenes is easily accomplished by changing the pH of the reaction mass.

Example 1. In a three-necked flask equipped with a droplet vortex, a reflux condenser, protected by chlorine-calcic tubes 11 with a mechanical stirrer, 5.61 g (17.84 lmuug) 1,3-d1yuxy-1,3-d11phenyldvinvinyldioylocoaia, 250 ml of dry toluene and 2 are placed , 82 g (35.68 mmol dry pyridine. From the dropping funnel, with stirring, pour over 30 shi-i 3.62 g (17.84 mmol) of phenylglycryldichlorosilane into 50 ml of dry toluene. Then, the reaction mass is heated with a light mild 3- 6 hours (until neutral but universal indicator). After cooling, hydrochloric acid Dine (99.5% of theoretically possible) is filtered off under a liquor and toluene is distilled off on a water-jet pump. The residue is distilled on a HpiH oil pump with a residual pressure of 1.5 mm Hg. 5.23 g are obtained (66% of theoretically possible tprfennltrivnnltsiklotrnsiloksana with so on. 160-165 ° C (1.5 mm Hg), which is a colorless oily liquid. Found,%: 65.03; 64.79; And 5.49 ; 5.61; S 19.03; 19.25; p, / 1.5545; 4 1.1149, 1.1124; MR 128.07; a pier weight. 448. S24I240z51z. P 5.44; Si 18.95; Calculated,%: C 64.82; MR “128.34; a pier weight 444.7. In the device described in Example 2, Measure 1, 4.28 g (13.61 mmol) of 1,3-dioxn-1, 3-diphenyldivine disdioxane, 250 ml of dry toluene and 2.15 g (27.22 mmol) of dry are placed. nrnd and-1a. 4.75 g (13.61 mmol) of 1,3-dlorchloro-1,3-difesh1livii11 ldisiloxane in 50 ml of dry toluene are added from the channel funnel with stirring for 30 minutes. Then, the reaction mass is heated by light boiling for 3-6 hours (until neutral but a universal indicator) and then treated with the procedure described in irimer 1. 4.60 g (57% of theoretically possible) tetraeleum tetrafennylnclotterasnloxan are obtained as a colorless oil liquid, quickly crystallized. %; C, 64.97; 65.18; H 5, 5.42; Paydeno, “,; 20 1,5587; t. kin. 238-240 ° C S 19.17; 1899. t. Pl. 142-143 ° C; a pier weight. 598. (1 mm Hg. Art.) Cz2Pz2O4514. C, 64.82; P 5.44; Si 18.95; Calculated,%; a pier weight. 592.8. The subject of the book is the art with the subsequent isolation of the target product by known irnemami.