Silicon tetrachloride → 3,7-Dimethyloctyl trichlorosilane

Temperature

-10 °C

Tetrahydrofuran (100 ml) and tetrachlorosilane (17.0 g, 100 mmol) were placed in a 500 mL four-necked flask in a nitrogen atmosphere, and cooled to −10° C. 3,7-dimethyloctyl magnesium bromide (Sigma-Aldrich Co. LLC., 1.0 M, 100 ml) was added dropwise, and the mixture was agitated for 1 hour at 10° C. or less. The temperature was raised gradually to room temperature over the course of about 1 hour, and the mixture was left standing overnight. The precipitated salt was filtered out, the tetrahydrofuran was removed by concentration under reduced pressure, and the mixture was distilled under reduced pressure to obtain the target 3,7-dimethyloctyl trichlorosilane (99-102° C./0.3 Torr, 22.3 g, yield 81%).

1. temperatureThe temperature was raised gradually to room temperature over the course of about 1 hour
2. waitthe mixture was left
3. waitstanding overnight
4. filtrationThe precipitated salt was filtered out
5. customthe tetrahydrofuran was removed by concentration under reduced pressure
6. distillationthe mixture was distilled under reduced pressure

ORD record

ord-441c85eb8e944551a7a488a1fe124ec7

Source dataset

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09212254B2