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 distillation under reduced pressure was performed 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, and distillation under reduced pressure

ORD record

ord-1f02370e1ccb49a49992d6a1e21e3503

Source dataset

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09212254B2