HRID515454

反应详情

EQUATION

反应方程式

HRID 515454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-(4-methoxy-benzyl)-6-methyl-[1,4]oxazepane (3.24 g, 13.8 mmol) in 1,2-dichloroethane (23 ml) was added 1-chloroethyl chloroformate (4.93 g, 34.5 mmol) at room temperature. The mixture was refluxed for 7 hours. The reaction mixture was cooled to room temperature and then methanol (30 ml) was added. The mixture was refluxed for 5 hours and concentrated in vacuo. This crude product was washed with hexane, dried under reduced pressure to afford 6-methyl-[1,4]oxazepane hydrochloride as white solid (1.73 g, 83%).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 7 hours
  2. temperatureThe mixture was refluxed for 5 hours
  3. concentrationconcentrated in vacuo
  4. washThis crude product was washed with hexane
  5. customdried under reduced pressure