HRID1979779

反应详情

EQUATION

反应方程式

HRID 1979779 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.0 Grams of 6-[3-(4-acetyl-4-phenyl-1-piperidyl)propoxy]-3,4-dihydrocarbostyril and 0.25 g of sodium hydride (50% in oil) were mixed in 30 ml of dimethylformamide and stirred for 1 hour, then 0.7 g of methyl iodide was added thereto and stirred at a room temperature for 12 hours. The reaction mixture was poured into 80 ml of saturated sodium chloride solution and the organic layer was extracted with chloroform and the chloroform layer was washed with water and dried. Then the chloroform was removed by distillation and the residue was crystallized with hexane. The crude crystals were recrystallized from ligroin to obtain 1.7 g of 1-methyl-6-[3-(4-acetyl-4-phenyl-1-piperidyl)propoxy]-3,4-dihydrocarbostyril as in the form of colorless needle-like crystals. Melting point: 115°-117° C.

WORKUP

后处理

  1. stirringstirred at a room temperature for 12 hours
  2. extractionthe organic layer was extracted with chloroform
  3. washthe chloroform layer was washed with water
  4. customdried
  5. customThen the chloroform was removed by distillation
  6. customthe residue was crystallized with hexane
  7. customThe crude crystals were recrystallized from ligroin