Dichlorodimethylsilane → HCID 131735714, compound

Temperature

80 °C

Under a nitrogen atmosphere, a 1-liter 3-necked flask equipped with a heating mantle, magnetic stirrer, pot thermometer, addition funnel and dry-ice condenser was charged with nonafluorohexyltrichlorosilane (457.8 g) and tetradecyl(trihexyl)phosphonium chloride (15.4 g). The mixture was heated to 80° C. and dimethylchlorosilane (124.9 g) was added to the mixture via addition funnel over 1 hr. The pot temperature dropped due to light chlorosilane refluxing. Upon completion of the addition, the reaction was refluxed for 6-8 hrs. The pot temperature slowly increased to 75° C., which indicates the conversion of dimethylchlorosilane to dimethyldichlorosilane. The reaction was cooled to room temperature and GC analysis (low-temp. method) of the mixture indicated about 84% completion. The pot was vented carefully under the protection of nitrogen. Distillation provided 386.6 g of crude product (63.5% pure, 58.0% yield).

1. customUnder a nitrogen atmosphere, a 1-liter 3-necked flask equipped with a heating mantle, magnetic stirrer
2. additionpot thermometer, addition funnel and dry-ice condenser
3. additionUpon completion of the addition
4. temperaturethe reaction was refluxed for 6-8 hrs
5. temperatureThe pot temperature slowly increased to 75° C.
6. temperatureThe reaction was cooled to room temperature
7. distillationDistillation

ORD record

ord-ebf9e7bc5fc54226a690d9d15f14b57b

Source dataset

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09359386B1