HRID4932

反应详情

EQUATION

反应方程式

HRID 4932 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 7-bromo-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid (8.53 g) dissolved in DMF (80 ml), were added potassium carbonate (13.8 g) and benzyl bromide (4.5 ml) and the mixture was stirred for 2 hours at room temperature. After the insoluble matter was filtered off and the filtrate was concentrated, a mixed liquid of ethyl acetate-benzene (1:1, 400 ml) was added to the residue, and the mixture was washed with water, dried over anhydrous sodium sulfate and then subjected to distilling off the solvent to give the intended compound 11.35 g (99.7%) as brown oily matter.

WORKUP

后处理

  1. filtrationAfter the insoluble matter was filtered off
  2. concentrationthe filtrate was concentrated
  3. additiona mixed liquid of ethyl acetate-benzene (1:1, 400 ml) was added to the residue
  4. washthe mixture was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationto distilling off the solvent