SU448720A1 - Method of producing sililmethyl trihaloide stannanes - Google Patents

Abstract

THE METHOD OF OBTAINING SIOILMETHIL-TRIGALOGENTANNANES by the interaction of C-halomethyl halidesilanes with anhydrous di-halide of divalent tin when heated to 100-200 * s, characterized by the fact that, in order to increase the target product, the process is carried out in the presence of one of the subjects of the subjects of the subjects of the subjects of the subjects of the subjects of subjects of the subjects of the subjects of the subjects of the subjects of the subjects of the subjects of the subjects of the subjects of the subjects of the subjects of the subjects of the subjects of the Teachers of the Teachers of the Teachers, in order to raise the figure of the Teachers of Teachers. 10-60 mol.% As a catalyst, in an inert atmosphere. A method according to Claim 1, characterized in that, in order to obtain compounds containing a Si-Hal bond, as the ω-halo-methylsilanes, take about & halo-methyl halo-silanes.

Description

This invention relates to the preparation of silylmethyltrigalogenstannans of the general formula. Hae R SiCH SnHae,. where R is alkyl, aryl, alkenyl, alkr or H, Hal is halogen, preferably chlorine or bromine, pi 0,1,2, which can be used as lubricants, hydraulic fluids, plasticizers, flame protective agents and coatings stabilizing additives and biologically active substances, as well as monomers for the preparation of various polymeric materials. A known method of producing silylmethyltrigalogenstannans of the general formula, 2SnHal} from divalent tin divalent (SnHal) and corresponding to the o-halomethylhalogenosilanes in a solvating solvent at a temperature of 100-200C. In this way, however, it is impossible to obtain a silyltyl hydrogen gage. since they interact with the solvent, the C – O bond is cleaved. The aim of the invention is to create a method that allows to obtain similar compounds containing Si-H bonds, as well as an increase in the yield of target products, which is achieved by carrying out the process in the presence of onium salts as a catalyst. A method for producing methyltrigalogenstannan forces is described, in which anhydrous divalent tin halide (ijnHal) is reacted with coi-halo methyl halide halide Ha1 (, Rj SiCHjHa in the presence of onium salts as catalyst at 100,200. C, ISO-lSO c, according to the Ho scheme (e (T, R SiCH, Hae49ttHaei) Various ammonium, phosphonium or other onium salts in the amount of 10-60 mol.%, Preferably 30-50 mol.%, Taken on SnHal are used as catalyst. lead in an autoclave or at atmospheric pressure in atmosphere (nitrogen, argon, etc.) with a molar ratio of ε-halo-methyl halo-silane and SnHalg from 1: 1 to 10: 1. The reaction time is 1-24 hours, usually 3-8 hours. as a diluent. It is advisable to use dihalo genide of tin and ω-halomethyl halo-silane with the same halogen, preferably with chlorine. At the same time, silylmethyltrigalogenstannans depending on the number of halogen atoms in silicon in the initial σ-halo-methyl halide silane, the conditions and time of the reaction are silicon, and the conditions and time of the reaction are equal to 29%. SnHal2. The silylmethyltrihalostannanes obtained are characterized by the fact that they contain from 4 to 6 extremely active halogen atoms in the molecule. Thankfully, the use of halosilylmethyltrihalostannans can be expected to open up even greater possibilities for practical use of this type of compounds, and derivatives based on them can have interesting properties that add properties derivatives based on silylmethyltrigalogenstannans that do not contain Si-Hal bonds. Example. 1. In a swinging autoclave with a capacity of 0.2 liters in a stream of nitrogen load 57 g (0.3 mol) of anhydrous SnCl2; 107.4 g (0.75 mol) of c6 chloromethyldimethylchlorosilane and 19.4 g (0.1 mol) of triethylbutylammonium chloride. The reaction mixture is heated under stirring for 6 hours. Then, after cooling the autoclave, its contents are transferred to a Klysen flask and dispersed. After distilling off the excess amount of the starting Oi-chloromethyldimethylchlorosilane by vacuum distillation, the fraction with so b.p. 130-13b C / a, 5 mm (, 5270), which by this gas-liquid chromatography, elemental analysis, IR and PMR spectrometry is pure dimethylchlorosilylmethyltrichlorstannane, C1 (CH j) 2S i CHjSn С 72 g (72, 3% for taken SnCl). Found,%: C 10.92 / H 2.44, C1 41.16, Si 9, Ol; Sn 34.93 .. C} H8SiSnCl4 Calculated,%: C 10.83; H 2.42 {C1 42.65, Si 8.44 ", Sn 35.66. Example2. Under conditions of example i, of 19 g (0.1 mol) of anhydrous SnCl,. 81 g (0.5 mol) of chloromethylmethyldichlorosilane and 9.8 g (0.05 mol) of triethylbutyl ammonium chloride in the presence of 50 ml of dry benzene give 26 g of methyldichlorosilylmethyl trichloromethane, Cl2 (CHJ) SiCH2SnCl, (73.5% yield, taken on taken, taken on a taken back ClCl (CHJ) SiCH2SnCl, 73.5% yield; -) t.kip. 101-108 ° C / 0.7 Kw (, 5043). Found,%: C 6.97; H 1.54, Cl 49.66; Si 7.81; Sn 32.92, CjjHySiSnClj Calculated: C 6.80 H 1.45 1 50.20; Si 7.95, Sn 33.60. Example Z.In the conditions of application 1 of 19 g (0.1 mol) of anhydrous

SnCl, 92 g (0.5 mol. Chloromethyl-trichlorosilane and 9.8 g (0/05 mol) of triethylbutylammonium chloride in the presence of 50 ml of dry heptane get 11 g of trichlorosilylmethyltrichlorstannane, CljSiCHgSnClj (29.8% yield from the taken CnCl2), m.p. 75-8b®С / 0,2 mm (nlf 1,5327).

Found%: C 3.57, H 0.78 / C1 55.77tSi 8.06; Sn 30.44, CHjSiSnSlg

Calculated,% C 3.23, H 0.55, Cl 56, 7.56, Sn 31.83.

Example 4. Under the conditions of example 1, out of 19 g (0.1 mol) of anhydrous SnCl2, 71.6 g (0.5 mol) of α-chloromethyl dimethylchlorosilane and 19.3 g (0.05 mol) of tetrabutyl phosphonium iodide

28.6 g of dimethylchloro-silyl-methyltrichlorstannane are obtained (yield 86% on taken SnClj).

Example 5. Under the conditions of example 1 out of 19 g (0.1 mol) anhydrous

SnCl, 49 g (0.4 mol) of flt-chloromethyltrimethylchlorosilane, 9.8 g (0.05 mol) of triethylbutylammonium chloride and 35 g of diethylene glycol dimethyl ether (28 g) give trimethylsily-

lilmethyltrichlorstannane. (CHj), (yield 89.5% on taken SnCl1) I b.p. 117-122 C / 20 mm (CG, 5152). Found,%: C 15.46} H 3.54,

C1 34, 9.12; Sn 37.85.

C4H |, SiSnCl4 Calculated,%: C 15.38 N 3.55J C1 34.06 jSi 8.99; Sn 38.01.

Claims (2)

METHOD FOR PRODUCING SICYLMETHYL TRIGALOGENSTANANS by the interaction of oC-halogenated methyl halosilanes with anhydrous tin dihalide when heated to 100-200 ^ 0, characterized in that, in order to increase the yield of the target products, the process is carried out in the presence of onium compounds taken in an amount of 10-60 mol. as a catalyst in an inert atmosphere. 2. The method according to π. 1, which involves the fact that, in order to obtain compounds containing a Si-Hal bond, β-halomethyl methyl halosilanes are taken as ob-halomethylsilanes.