반응 #1964656

반응 방정식

2-fluoro-4-[4-(quinolin-3-yl)-9H-carbazol-9-yl]benzonitrile

potassium carbonate

sodium hydroxide

hydrogen peroxide

4-amino-2(R,S)-methylbutanol

→

4-[4-(quinolin-3-yl)-9H-carbazol-9-yl]-2-(4-hydroxy-3(R,S)-methylbutylamino)benzamide

용매

dimethyl sulphoxide

ethanol

반응 조건

후처리

1. 1
   기타obtained
2. 2
   기타After treatment as in stage 3 of Example 3, and then purification by flash chromatography
3. 3
   세척on silica gel, elution
4. 4
   workup.ADDITIONbeing carried out with a mixture of dichloromethane and ethanol (95/5 by volume)
5. 5
   기타followed by crystallization from 5 ml of ethyl acetate, 225 mg of 4-[4-(quinolin-3-yl)-9H-carbazol-9-yl]-2-(4-hydroxy-3(R,S)-methylbutylamino)benzamide
6. 6
   기타are thus obtained in the form of a beige solid

실험 절차

The process is carried out as in stage 2 of Example 3, but using 300 mg of 2-fluoro-4-[4-(quinolin-3-yl)-9H-carbazol-9-yl]benzonitrile, obtained according to stage 1 of Example 32, 301 mg of potassium carbonate and 1.50 g of 4-amino-2(R,S)-methylbutanol in 3 ml of dimethyl sulphoxide. 1.38 ml of a 1M aqueous solution of sodium hydroxide, 1.336 ml of a 30% aqueous solution of hydrogen peroxide and 7 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 (95/5 by volume), followed by crystallization from 5 ml of ethyl acetate, 225 mg of 4-[4-(quinolin-3-yl)-9H-carbazol-9-yl]-2-(4-hydroxy-3(R,S)-methylbutylamino)benzamide are thus obtained in the form of a beige solid, the characteristics of which are the following:

출처