Trichloro(1,1,2,2,3,3,6,6,6-nonafluorohexyl)silane

Conditions: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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). 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 Upon completion of the addition the reaction was refluxed for 6-8 hrs The pot temperature slowly increased to 75° C. The reaction was cooled to room temperature Distillation