HRID2251937

反应详情

EQUATION

反应方程式

HRID 2251937 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20.0 g (89.5 mmol) 1-phenyl-1,2,4,5-tetrahydrobenzo[d]azepine, 25.2 g (89.5 mmol) N-(4-bromobutyl)-phthalimide and 18.5 g (134.3 mmol) potassium carbonate are stirred in 200 ml DMF for 6 hours at 60° C. The mixture is concentrated under vacuum and the residue is distributed between 300 ml acetic acid ethyl ester and 100 ml water. The watery phase is extracted with 50 ml acetic acid ethyl ester and the combined organic phases are washed with water. The organic phase is dried over sodium sulfate and evaporated under vacuum until dried: Yield 39.5 g.

WORKUP

后处理

  1. concentrationThe mixture is concentrated under vacuum
  2. extractionThe watery phase is extracted with 50 ml acetic acid ethyl ester
  3. washthe combined organic phases are washed with water
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. customevaporated under vacuum
  6. customuntil dried