HRID1667316

反应详情

EQUATION

反应方程式

HRID 1667316 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customThe reaction mixture was evaporated under reduced pressure
  2. distillationthe residue was azeotropically distilled with 5 ml of toluene 3 times
  3. customto give crystals
  4. customThe collected crystals were recrystallized from ethanol-ethyl acetate