反应 #1869177
ord-47698fe631f744f7bb78fc6f4bd9c905
反应方程式
4-piperidone hydrochloride monohydrate
benzyloxycarbonyl chloride
hydrochloric acid
→
title compound
收率 100.3%
N-benzyloxycarbonyl-4-piperidone
收率 100.3%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1萃取the aqueous solution was extracted three times with ethyl acetate
- 2洗涤The organic layer was washed with a saturated aqueous solution of sodium bicarbonate
- 3干燥a saturated aqueous solution of sodium chloride subsequently, dried over anhydrous magnesium sulfate
- 4浓缩concentrated
实验过程
A 4-piperidone hydrochloride monohydrate (15.3 g) was dissolved in 2N aqueous solution of sodium hydroxide (100 mL). To the solution was added a benzyloxycarbonyl chloride (20.4 g) at 0° C. The mixture was stirred for 1 hour. The reaction mixture was neutralized with 2N hydrochloric acid, and the aqueous solution was extracted three times with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride subsequently, dried over anhydrous magnesium sulfate and concentrated to give the title compound (23.3 g) having the following physical data.