HCID 57370488, compound → HCID 131736726, compound

Participants

Reaction Steps

A stainless steel pressure vessel equipped with a thermometer, a stirrer, and a condenser was charged with 53.6 g (0.4 mol) of dimethoxymethylsilane, 67.2 g (0.42 mol) of dimethoxymethylvinylsilane, and 0.5 ml of a 0.1 mol/l solution of chloroplatinic acid in isopropyl alcohol. The vessel was closed, and the contents were heated while stirring at 80° C. for 30 minutes. After completion of the reaction, the reaction mixture was distilled to give 88.4 g of a mixture of 1,2-bis(dimethoxymethylsilyl)ethane and 1,1-bis(dimethoxymethylsilyl)ethane. To a PFA reactor equipped with a thermometer, a stirrer, and a condenser were put 76.8 g (a total of 0.3 mol) of the mixture as obtained above and 50 g of cyclopentane. While cooling the reactor with water to 0° to 10° C., 58.7 g (1.35 mol) of 46% aqueous hydrofluoric acid was added thereto dropwise. After the dropwise addition, the stirring was continued for 2 hours at 30° C. to complete the reaction. The reaction solution was allowed to stand, and the separated aqueous layer was removed. The organic layer was washed with a saturated sodium chloride aqueous solution and evaporated to give 44.7 g of a mixture containing 70% 1,2-bis(difluoromethylsilyl)ethane and 30% 1,1-bis(difluoromethylsilyl)ethane (designated mixture A2). The 1,2-bis(difluoromethylsilyl)ethane is a compound of general formula (1) in which R1 and R2 are both methyl, and the 1,1-bis(difluoromethylsilyl)ethane is a compound of general formula (2) in which R3 and R4 are both methyl.

Provenance & Evidence