SU445671A1 - The method of obtaining phenyltrichlorhex or its derivatives, containing substituents in the aromatic ring - Google Patents

Description

one

This invention relates to a process for the preparation of phenyltrichlorogerman or its derivatives, containing substituents in the benzene ring, which are used in preparative chemistry.

A known method for producing phenyltrichlorogermann or its derivatives containing substituents on the aromatic ring by reacting phenyl silicon compounds, for example phenyltrichlorosilane, with tetrachloride germanium in the presence of aluminum chloride as a catalyst at elevated temperature.

The disadvantages of this method are the insufficiently high yield of the target products and the relatively high consumption of catalyst.

The purpose of the invention is to increase the yield of the target products and reduce the consumption of the catalyst - achieved by using alkylphenylchlorosilane, or its derivative, containing its substituent in the aromatic ring as the phenyl compound of silicon.

The reaction is usually carried out at 100-150 ° C in the presence of not more than 0.3 mol of aluminum chloride per 1 mol of chlorosilane.

. Output target products 66-91%.

Example 1. 191 g (1 mol) of phenylmethyldichlorosilane and 225.2 g (1.05 mol) of germanium tetrachloride are placed into a cube of a glass distillation column (10 t. T.) With a glass nozzle and 40 g (0 , 3 mol) aluminum chloride,

2 hours are heated to 100 ° C and start sampling through the top of the methyltrichlorosilane column (bp 65 ° C) at a reflux ratio of 15. The selection is continued for 6 hours at a temperature B cube of the column 100 ° C, after which the temperature is raised to 120 ° C to terminate the reaction, continuing the selection of methyl trichlorosilane. After cooling, the alumina chloride is separated from the reaction mixture of the mixture, the residue is distilled, and 232 g of phenyltrichlorohermann are obtained.

t. kin. 97 ° C / 10 mm; 1.5951; by

, 5545.

Example 2. Analogously to Example 1, a mixture of 225.8 g (1 mol) of chlorophenylmethyl dichlorosilane, 225.2 g (1.05 mol) of germanium tetrachloride and 40 g (0.3 mol) of aluminum chloride is heated to 5 ° C (the reaction starts temperature 2 hours after the start of heating), after 8 hours, heated to 130 ° C and kept for 4 hours at 130 ° C. Methyltrichlorosilane is taken all the time during heating. At the end of the reaction, aluminum chloride is separated, the residue is distilled, and 261 g (90%) of chlorofenpltrichlorogermanm are obtained.

m.p. 118/120 ° C / 10mm; Y20 1,6891; by 1.5700. Froze As in example 1, a mixture of 110 g

Bromophenylmethyldichlorosilane, 90 g of germanium tetrachloride and 16 g of aluminum chloride are heated to 120 ° C, kept at this temperature for 2 hours, heated to 130 ° C, and the mixture is kept at GSO-135 ° C for 10 hours, the methyltrichlorosilane formed is heated during heating. At the end of the reaction, aluminum chloride is separated, the residue is distilled, and 90 g (66%) of bromophenyltrichlorogermanm is isolated, i.e. bale. 115-120 ° C / 4 mm; H20 2,0434; "At 1.6040.

Subject invention

Claims (3)

1. A method of producing phenyltrichloroermann or its derivatives containing substituents on the aromatic ring, by reacting phenyl silicon compounds with germanium tetrachloride in the presence of aluminum chloride at an elevated temperature, characterized in that, in order to increase the yield of the target products and reduce the consumption of the catalyst, as phenyl silicon compounds use alkylphenylchlorosilane or a derivative thereof containing a substituent on the aromatic ring. 2. A process according to claim 1, characterized in that no more than 0.3 mol of aluminum chloride is used per 1 mol of chlorosilane. 3. A method according to claim 1, characterized in that the process is carried out at 100-150 ° C.