反应 #3277308
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06994800B1
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Lithium bis(ethyldimethylsilyl)amide was prepared by the slow addition via syringe of a hexane solution of butyl lithium (50.6 mL of 2.73 M solution, 138 mmol) to a stirred hexane solution (100 mL) of bis(ethyldimethylsilyl)amine (26.2 g, 138 mmol) at room temperature. Stirring was continued for one hour and the solution was then refluxed for one hour. The hexane was evaporated under vacuum, leaving a pale yellow liquid. It was distilled at a temperature of 123° C. and a pressure of 0.2 torr to yield 23.2 g (86%) of clear liquid lithium bis(ethyldimethylsilyl)amide. Its viscosity was measured to be 37.5 centipoise at 40° C. Its NMR parameters are as follows: the solution was then refluxed for one hour The hexane was evaporated under vacuum leaving a pale yellow liquid It was distilled at a temperature of 123° C.
来源 ID: ord-1e36c61fa6114ead93486d0ec4e78ad6