HRID1285437

反应详情

EQUATION

反应方程式

HRID 1285437 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.0 Grams of 6-{1-oxo-4-[4-(3-chlorophenyl)-1-piperazinyl]butyl}-3,4-dihydrocarbostyril was added to 100 ml of methanol, under stirring condition 1.2 g of sodium borohydride was added gradually to the solution and stirred at a room temperature for 5 hours. Then 5 ml of concentrated hydrochloric acid was added to the reaction mixture and the mixture was concentrated under a reduced pressure to dryness. Then to this dried matter was added 50 ml of 2%-sodium hydroxide aqueous solution and the organic layer was extracted with dichloromethane. The dichloromethane layer was washed with water, dried and the dichloromethane was removed by distillation. The residue thus obtained was purified by a silica gel column chromatography, and recrystallized from isopropanol to obtain 2.2 g of 6-{1-hydroxy-4-[4-(3-chlorophenyl)-1-piperazinyl]butyl}-3,4-dihydrocarbostyril in colorless needle-like crystals.

WORKUP

后处理

  1. additionwas added gradually to the solution
  2. concentrationthe mixture was concentrated under a reduced pressure to dryness
  3. additionThen to this dried matter was added 50 ml of 2%-sodium hydroxide aqueous solution
  4. extractionthe organic layer was extracted with dichloromethane
  5. washThe dichloromethane layer was washed with water
  6. customdried
  7. customthe dichloromethane was removed by distillation
  8. customThe residue thus obtained
  9. customwas purified by a silica gel column chromatography
  10. customrecrystallized from isopropanol