HRID1646902

反应详情

EQUATION

反应方程式

HRID 1646902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirring solution of 5.23 g (20 mmol) of 8-chlorodibenzo[b,f][1,4]thiazepin-11(10H)-one (34), prepared in the manner described above in Example 34, in 175 mL of THF cooled in an ice bath is added dropwise 100 mL of M lithium aluminum hydride solution. The reaction is heated at reflux for 4 hours. The reaction is quenched by the addition of 3.8 mL of 15% NaOH and 15.2 mL of H2O. The reaction mixture is filtered through a pad of celite. The filtrate is concentrated in vacuo and is recrystallized from cyclohexane.

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. temperatureThe reaction is heated
  3. temperatureat reflux for 4 hours
  4. customThe reaction is quenched by the addition of 3.8 mL of 15% NaOH and 15.2 mL of H2O
  5. filtrationThe reaction mixture is filtered through a pad of celite
  6. concentrationThe filtrate is concentrated in vacuo
  7. customis recrystallized from cyclohexane