二氯-双[(2-甲基丙-2-基)氧基]硅烷

反应条件: temp:-20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 20 g (0.0799 mol) of bis(tert-butoxy)dichlorosilane prepared by reaction of SiCl4 with two equivalents of tert-butanol in the presence of pyridine was loaded in a 1000 ml three-neck flask with 200 ml hexane. The flask was cooled down to −20° C. with a cold bath containing dry ice and iso-propanol. 4.8 g (0.08 mol) of iso-propanol was added. The temperature was kept at less than −20° C. 6.3 g of pyridine was added to the flask slowly to generate a lot of white precipitate, which is pyridine.HCl. The cold bath was removed and the flask was stirred for several days at room temperature after removal of the cold bath. Filtration and removal of solvents resulted in white slurry. The white slurry was dropwise added to a solution containing 50 ml of ether, 50 ml of water, and 6 g of NH4.HCO3 at a temperatue below −10° C. until completion of the addition. The resulting white slurry was stirred overnight. The organic layer was separated and dried over anhydrous CaCl2. GC/MS indicated the formation of bis(tert-butoxy)(iso-propooxy)silanol as the major product (93.8%), plus bis(tert-butoxy)(iso-propoxy)chlorosilane. Vacuum distillation gives pure bis(tert-butoxy)(iso-propoxy)silanol (˜104° C./2 torr). was kept at less than −20° C The cold bath was removed after removal of the cold bath Filtration and removal of solvents resulted in white slurry The white slurry was dropwise added to a solution HCO3 at a temperatue below −10° C. until completion of the addition The resulting white slurry was stirred overnight The organic layer was separated dried over anhydrous CaCl2 Vacuum distillation