Dichloromethylphenylsilane → HCID 131729656, Verbindung

Temperatur

50 °C

To a round flask (internal volume: 1000 ml) equipped with a three-way stopcock, 90 g of granular magnesium (particle size: 20 to 1000 μm) and 20 g of lithium chloride as a catalyst were fed, and the internal of the reaction vessel (flask) was dried with heating at 50° C. under a reduced pressure of 1 mmHg (=133 kPa). Thereafter, dry argon gas was introduced into the reaction vessel, 500 ml of tetrahydrofuran (THF) pre-dried with sodium-benzophenone ketyl was added thereto, and the mixture was stirred at 25° C. for about 60 minutes. To the reaction mixture were added 114.7 g (0.6 mol) of methylphenyldichlorosilane purified by distillation and 35.4 g (0.2 mol) of phenyldichlorosilane purified by distillation by the use of a syringe, and the resulting mixture was stirred at 25° C. for about 24 hours. After completion of the reaction, 2000 ml of 1N (=μmol/L) hydrochloric acid was put in the reaction mixture, and the reaction mixture was subjected to extraction with 500 ml of toluene. The washing of the toluene layer with 200 ml aliquots of purified water was repeated ten times, and the toluene layer was dried with anhydrous magnesium sulfate, and then toluene was distilled off to give a methylphenyldichlorosilane-phenyldichlorosilane copolymer (the former/the latter (molar ratio)=3/1) (weight-average molecular weight: 4000).

1. customthe internal of the reaction vessel (flask) was dried
2. additionThereafter, dry argon gas was introduced into the reaction vessel, 500 ml of tetrahydrofuran (THF)
3. dry with materialpre-dried with sodium-benzophenone ketyl
4. additionwas added
5. distillationpurified by distillation by the use of a syringe
6. stirringthe resulting mixture was stirred at 25° C. for about 24 hours
7. customAfter completion of the reaction, 2000 ml of 1N (=μmol/L) hydrochloric acid
8. extractionthe reaction mixture was subjected to extraction with 500 ml of toluene
9. washThe washing of the toluene layer with 200 ml aliquots of purified water
10. dry with materialthe toluene layer was dried with anhydrous magnesium sulfate
11. distillationtoluene was distilled off

ORD-Eintrag

ord-7124374a0d7b4ad58850038c03021954

Quelldatensatz

uspto-grants-2012_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08163863B2