反应详情

To a suspension of 79 mg (0.45 mmol) of 6-amino-1H-indole-7-carboxylic acid in 7 mL of acetonitrile, is added 130 mg (0.45 mmol) of 2-(3-chloro-pyridin-2-yl)-5-trifluoromethyl-2H-pyrazole-3-carboxylic acid followed by 0.16 mL (2.06 mmol) of pyridine. The mixture is stirred at ambient temperature during 30 minutes. Then the suspension is cooled to 0° C. and 0.12 mL (1.57 mmol) of methanesulfonyl chloride is added dropwise. The mixture is stirred at 0° C. during 30 minutes and 2 hours at ambient temperature. After evaporation of the solvent, the residue is triturated with a minimum of cold water. The precipitate which is formed is filtrated and washed with cold water. The residue is then purified by column chromatography on silica gel with hexanes and ethyl acetate as eluents and 47.1 mg (0.11 mmol, 25%) of a yellowish solid are obtained; LC/MS:432/434 (M+H)+.

1. temperatureThen the suspension is cooled to 0° C.
2. stirringThe mixture is stirred at 0° C. during 30 minutes and 2 hours at ambient temperature
3. customAfter evaporation of the solvent
4. customthe residue is triturated with a minimum of cold water
5. customThe precipitate which is formed
6. filtrationis filtrated
7. washwashed with cold water
8. customThe residue is then purified by column chromatography on silica gel with hexanes and ethyl acetate as eluents