HRID1263102

反应详情

EQUATION

反应方程式

HRID 1263102 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.0 Grams of 6-(4-chloro-1-oxobutyl)-3,4-dihydrocarbostyril was disposed in 200 ml of methanol, and the suspension was stirred at a room temperature. Then 2.0 g of sodium borohydride was added to the suspension gradually and the reaction was continued for 1 hour. Next, 3 ml of concentrated hydrochloric acid was added to the reaction mixture and the mixture was concentrated under a reduce pressure with heat-refluxing condition to obtain a residue. The residue was extracted with chloroform and the chloroform layer was washed with water and dried. Then chloroform was removed by distillation under a reduced pressure to obtain a residue, and the residue was recrystallized from ethanol to obtain 2.4 g of 6-(4-chloro-1-butenyl)-3,4-dihydrocarbostyril in yellow needle-like crystals. Melting point: 153°-155° C.

WORKUP

后处理

  1. concentrationthe mixture was concentrated under a reduce pressure
  2. temperaturewith heat-refluxing condition
  3. customto obtain a residue
  4. extractionThe residue was extracted with chloroform
  5. washthe chloroform layer was washed with water
  6. customdried
  7. customThen chloroform was removed by distillation under a reduced pressure
  8. customto obtain a residue
  9. customthe residue was recrystallized from ethanol