HRID272095
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 7.96 g of {(3S)-1-(tert-butoxycarbonyl)-3-piperidyl}methanol in 150 ml of chloroform, 3.4 ml of methanesulfonyl chloride and 6.7 ml of triethylamine were added under cooling with ice, followed by an hour's stirring at room temperature. The reaction liquid was distilled off under reduced pressure, diluted with ethyl acetate and saturated aqueous sodium bicarbonate solution was added, followed by 1.5 hours' stirring. Thereafter the reaction liquid was successively washed with water and saturated brine and dried over anhydrous magnesium sulfate. Distilling the solvent off, 10.50 g of the title compound was obtained.
WORKUP
后处理
- temperatureunder cooling with ice
- waitfollowed by an hour
- customThe reaction liquid
- distillationwas distilled off under reduced pressure
- additiondiluted with ethyl acetate and saturated aqueous sodium bicarbonate solution
- additionwas added
- stirring' stirring
- customThereafter the reaction liquid
- washwas successively washed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- distillationDistilling the solvent off, 10.50 g of the title compound
- customwas obtained