HRID1877504

反应详情

EQUATION

反应方程式

HRID 1877504 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The process is carried out as in stage 3 of Example 3, but using 165.4 mg of 2-fluoro-4-[4-(quinolin-3-yl)-9H-carbazol-9-yl]benzonitrile, obtained according to stage 1 of Example 32, 165.8 mg of potassium carbonate and 356 mg of 4-aminomethyl-1-methyl-1H-pyrazole in 1.7 ml of dimethyl sulphoxide, in a microwave for 1 hour and 30 minutes at 115° C. 0.76 ml of a 1M aqueous solution of sodium hydroxide, 0.735 ml of a 30% aqueous solution of hydrogen peroxide and 4 ml of ethanol are then added to the reaction medium. After treatment as in stage 3 of Example 3, and then purification by flash chromatography on 10 g of silica gel, elution being carried out with a mixture of dichloromethane and methanol (95/5 by volume), 2-[(1-methyl-1H-pyrazol-4-yl)methylamino]-4-[4-(quinolin-3-yl)-9H-carbazol-9-yl]benzamide is thus obtained in the form of a white powder, the characteristics of which are the following:

WORKUP

后处理

  1. customobtained
  2. customAfter treatment as in stage 3 of Example 3, and then purification by flash chromatography
  3. washon 10 g of silica gel, elution
  4. additionbeing carried out with a mixture of dichloromethane and methanol (95/5 by volume), 2-[(1-methyl-1H-pyrazol-4-yl)methylamino]-4-[4-(quinolin-3-yl)-9H-carbazol-9-yl]benzamide
  5. customis thus obtained in the form of a white powder