HRID1877489

反应详情

EQUATION

反应方程式

HRID 1877489 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 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

  1. customobtained
  2. customAfter treatment as in stage 3 of Example 3, and then purification by flash chromatography
  3. washon silica gel, elution
  4. additionbeing carried out with a mixture of dichloromethane and ethanol (90/10 by volume)
  5. 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
  6. customare thus obtained in the form of a beige solid