HRID1646902
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 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
- temperaturecooled in an ice bath
- temperatureThe reaction is heated
- temperatureat reflux for 4 hours
- customThe reaction is quenched by the addition of 3.8 mL of 15% NaOH and 15.2 mL of H2O
- filtrationThe reaction mixture is filtered through a pad of celite
- concentrationThe filtrate is concentrated in vacuo
- customis recrystallized from cyclohexane