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 150 mg of 2-fluoro-4-[4-(quinolin-3-yl)carbazol-9-yl]benzonitrile, obtained according to stage 1 of Example 32, 150.5 mg of potassium carbonate, 1.336 g of 2-(1H-imidazol-1-yl)ethylamine dihydrochloride in 2 ml of dimethyl sulphoxide. 0.69 ml of a 1M aqueous solution of sodium hydroxide, 0.667 ml of a 30% aqueous solution of hydrogen peroxide and 3 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 silica gel, elution being carried out with a mixture of dichloromethane and ethanol (90/10 by volume), followed by crystallization from 1 ml of ethyl acetate and 3 ml of diisopropyl ether, 130 mg of 2-[2-(1H-imidazol-1-yl)ethylamino]-4-[4-(quinolin-3-yl)-9H-carbazol-9-yl]benzamide are thus obtained in the form of a beige solid, 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 silica gel, elution
- additionbeing carried out with a mixture of dichloromethane and ethanol (90/10 by volume)
- customfollowed by crystallization from 1 ml of ethyl acetate and 3 ml of diisopropyl ether, 130 mg of 2-[2-(1H-imidazol-1-yl)ethylamino]-4-[4-(quinolin-3-yl)-9H-carbazol-9-yl]benzamide
- customare thus obtained in the form of a beige solid