SU375933A1 - METHOD FOR OBTAINING 1,7-BIS- (HYDROXYTETRAORGANOSYOXANYL) -CARBORANE 12 The invention relates to the field of producing hydroxyl-containing organosilicon derivatives of carboran. which can be used as monomers for the synthesis of carboransiloxane polymers. A method is known for producing siloxanilcarboranes, in particular, 1.7-b "c- (hydroxytetraorgano-siloxanil) -carborane with the general formula 5: BUT - V.? ^? SiO-Sl-CB, oH, oC-Si-0-StO 1 I '' '',} [Л ЕR R •• В - Google Patents

Description

where p ":; 10, by hydrolysis of 1,7-bis- (chlorotetraorganosiloxanil) -carborane in an acidic medium when heated, for example, to 100 ° C.

However, due to the fact that, using a known method, only dichloro-tetraorganosiloxanilcarborane is used as the starting compound, the hydrolysis process takes place in the presence of liberated hydrogen chloride, which does not allow to isolate individual 1,7-B1NC- {hydroxytetraorganosiloxanil) -carborane, and results in oligomers containing 10 links. This product, which is a mixture of diols of different molecular weights, is almost impossible to control for purity.

CH R

Gh.

R

one

X-Si-O-Si-GBjoHjoC-Si-O-Si-X-fHz OCHj CiHjCHj GHj

The purpose of the invention is to obtain hydroxyl-containing organosilicon derivatives of carboran with a high degree of purity, suitable for the synthesis of carboransiloxane elastomers.

The problem was solved by hydrolysis of 1.7by- (alkoxy- or acyloxytetra-organosiloxanil) -carboranes.

According to the proposed method, 1,7-bass- (alkoxy- or acyloxytetra-organosiloxanil) -carboranes are hydrolyzed in the presence of an organic acid, for example acetic acid, when heated according to the scheme

in CH ,, CHj R

-HOSi-U-Si-CBiuHioG-Si-U-Si-UH + mX

CHb CHs

CHz CHj

where X is an alkoxy or acyloxy group; R is alkyl or aryl.

The reaction is carried out at 80-100 ° C for 1.5-2 hours. The formed 1.7b "c- (hydroxytetraorganosiloxanyl) -carborane of high purity was isolated in 96-99% quantitative yield using known methods.

Example. 1. In a flask equipped with a stirrer and reflux condenser, 14.59 g (0.0279 mol) of 1.7-byc- (acetoxytetramethylsiloxanil) -carborane and 80 ml of water are charged. The reaction mixture is stirred at 80-100 ° C for 1.5-2 hours. The final product is dried at 100 ° C under vacuum (4-5 mm Hg. Art.).

11.73 g (96.5% yield) of 1.7-b c (hydroxytetramethylsiloxanil) -carborane are obtained.

The content of OH groups,%: found 7,69, calculated 7,77. T. pl. 48-48.5 ° C; df 1.0278; MRo found 124.33; MRc calculated 124.13.

Example 2. In a flask equipped with a stirrer and reflux condenser, load 3.12 g (0.0067 mol) 1.7-bis- (methoxytetramethylsiloxanil) -carborane, 6.4 ml of water, 12.8 ml of ethyl alcohol and 0, 5 ml of acetic acid. Synthesis is carried out according to Example 1.

2.78 g (95% yield) of 1.7-byc- (hydraxite-tramethylsiloxanil) -carborane is obtained.

Example 3. In a flask equipped with a stirrer and reflux condenser, 4.41 g (0.0068 mol) of 1.7-by-c (1,1,3-trimethyl-3 acetoxy-3-phenylsiloxanil) -carborane and 40 ml of water are charged. . Synthesis is carried out according to Example 1.

3.68 g (96% of theory) of 1.7-bis- (1,1,3-trimethyl-3-hydroxy-3-phenyl siloxanil) -carborane are obtained; p 1.5462.

The content of OH groups,%: found 6.03, calculated 6.04.

Subject invention

The method of obtaining 1.7-b "c- (hydroxytetraorganosiloxanil) -carborane by hydrolysis of the derivative 1,7-bis- (tetraorganosiloxanil) carboran in an acidic medium with heating, characterized in that, in order to obtain final products with a high degree of purity, as 1.7-bys- (tetra-organosiloxanil) -carborane derivative, use 1,7-bms- (alkoxy- or acyloxytetra-organosiloxanil) -carborane.