HRID395864
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 stirring solution of 1-Boc-4-methoxycarbonyl-3,4-didehydropiperidine (28.81 g, 119 mmol) in methanol (300 mL) was added 1 N aqueous sodium hydroxide (300 mL). After stirring overnight, the solvent was removed by rotary evaporation and the residue was partitioned between water and diethyl ether. The aqueous phase was separated and washed with diethyl ether, acidified to pH 2.5 with conc. HCl, then extracted with diethyl ether. The organic extract was then washed with brine, dried with MgSO4, filtered and concentrated in vacuo to give 25.16 g (93%) of a light yellow solid.
WORKUP
后处理
- customthe solvent was removed by rotary evaporation
- customthe residue was partitioned between water and diethyl ether
- customThe aqueous phase was separated
- washwashed with diethyl ether
- extractionextracted with diethyl ether
- extractionThe organic extract
- washwas then washed with brine
- dry with materialdried with MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo