HRID1733979

反应详情

EQUATION

反应方程式

HRID 1733979 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a slurry of 0.170 g of 1,4,5,6-tetrahydro-6-(4-nitrobenzoyl)pyrazolo[3,4-d]pyrido[2,3-b]azepine in 8 ml of ethanol under argon is added 0.573 g of stannous chloride dihydrate (SnCl2.2H2O). The mixture is refluxed for 1 hour, diluted with ice-water and made basic with 10% NaHCO3 solution. The mixture is stirred 3.5 hours and extracted with chloroform (3 times). The extract is dried (MgSO4) and the solvent removed under vacuum. Chromatography on silica gel with ethyl acetate as eluent gives 0.10 g of off-white crystals.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 1 hour
  2. extractionextracted with chloroform (3 times)
  3. dry with materialThe extract is dried (MgSO4)
  4. customthe solvent removed under vacuum