HRID1759312

反应详情

EQUATION

反应方程式

HRID 1759312 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.3 g (0.03 mole) of 6-hydroxy-2,3,4,5-tetrahydro-1H-benzazepin-2-one, 5 ml of epibromohydrin and 4.5 g of potassium carbonate in 250 ml of methyl isobutyl ketone are refluxed for 48 hours. After the mixture has cooled, it is filtered and the filtrate is concentrated under reduced pressure on a rotary evaporator. The residue is recrystallized from cyclohexane in the presence of animal charcoal. 4.2 g (60% yield) of 6-(2,3-epoxy-propoxy)-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one, of melting point 121°-123° C., are obtained.

WORKUP

后处理

  1. temperatureAfter the mixture has cooled
  2. filtrationit is filtered
  3. concentrationthe filtrate is concentrated under reduced pressure on a rotary evaporator
  4. customThe residue is recrystallized from cyclohexane in the presence of animal charcoal