HRID1667316
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 645 mg of tert-butyl 4-[(E)-2-(2-chloro-6-methylphenyl)vinyl]piperidine-1-carboxylate in 4 ml of ethanol, 3 ml of 35% hydrogen chloride-ethanol was added, followed by stirring at ambient temperature for 5 hours. The reaction mixture was evaporated under reduced pressure and the residue was azeotropically distilled with 5 ml of toluene 3 times to give crystals. The collected crystals were recrystallized from ethanol-ethyl acetate to give 377 mg of 4-[(E)-2-(2-chloro-6-methylphenyl)vinyl]piperidine hydrochloride.
WORKUP
后处理
- customThe reaction mixture was evaporated under reduced pressure
- distillationthe residue was azeotropically distilled with 5 ml of toluene 3 times
- customto give crystals
- customThe collected crystals were recrystallized from ethanol-ethyl acetate