HRID412518

反应详情

EQUATION

反应方程式

HRID 412518 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To an ethanol solution (2 ml) of 7-[1-(pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline-2-carbothioimidic acid methyl ester (100 mg) were added methylamine hydrochloride (20 mg) and sodium acetate (25 mg), and the mixture was stirred at 80° C. for 3 hours. After completion of the reaction, water was added and the mixture was washed with chloroform. Thereto was added aqueous sodium hydrogencarbonate solution and the mixture was washed with chloroform. To the aqueous layer was added 4N aqueous sodium hydroxide solution and the mixture was extracted with chloroform. The extract was washed successively with water and saturated brine. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated and the obtained residue was treated with hydrogen chloride—ethanol solution and dried under reduced pressure to give the title compound (80 mg).

WORKUP

后处理

  1. additionwas added
  2. washthe mixture was washed with chloroform
  3. additionThereto was added aqueous sodium hydrogencarbonate solution
  4. washthe mixture was washed with chloroform
  5. additionTo the aqueous layer was added 4N aqueous sodium hydroxide solution
  6. extractionthe mixture was extracted with chloroform
  7. washThe extract was washed successively with water and saturated brine
  8. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  9. customthe solvent was evaporated
  10. additionthe obtained residue was treated with hydrogen chloride—ethanol solution
  11. customdried under reduced pressure