反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customobtained
- customAfter treatment as in stage 3 of Example 3, and then purification by flash chromatography
- washon 10 g of silica gel, elution
- 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
- customis thus obtained in the form of a white powder