HRID409605
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 mixed solution containing 33.5 g of 3-hydroxypiperidine and 62.7 ml of triethylamine dissolved in 250 ml of methylene chloride was added dropwise a solution of 55.7 ml of benzyloxycarbonyl chloride in 150 ml of methylene chloride, and the mixture was stirred at room temperature for 16 hours. To the reaction mixture were added a saturated aqueous citric acid and chloroform, the mixture was stirred and the liquids were separated. The organic layer was dried, the solvent was evaporated, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=4→0:1) to obtain 75.5 g of benzyl 3-hydroxypiperidine-1-carboxylate.
WORKUP
后处理
- stirringthe mixture was stirred
- customthe liquids were separated
- customThe organic layer was dried
- customthe solvent was evaporated
- customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=4→0:1)