反应详情

To a suspension of 1.00 g (4.58 mmol) of 6-amino-5-chloro-1H-indazole-7-carboxylic acid in 40 mL of anhydrous acetonitrile is added 1.18 g (4.58 mmol) of 5-chloro-2-(3-chloro-pyridin-2-yl)-2H-pyrazole-3-carboxylic acid followed by 1.7 mL (20.6 mmol) of pyridine. The mixture is stirred at ambient temperature during 30 minutes. Then the suspension is cooled to 0° C. and 1.25 mL (16.0 mmol) of methanesulfonyl chloride is added dropwise. The mixture is stirred at ambient temperature for 6 hours. Then the solvent is evaporated and the residue is triturated with a minimum of cold water. The precipitate, which is formed is filtrated, washed with cold water and dried. Purification by flash chromatography (SiO2, toluene/methylene chloride/ethyl acetate 10:10:3) affords 910 mg (39%) of the product as a yellowish solid; LC/MS:433/435 (M+H)+.

1. temperatureThen the suspension is cooled to 0° C.
2. stirringThe mixture is stirred at ambient temperature for 6 hours
3. customThen the solvent is evaporated
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. customdried
9. customPurification by flash chromatography (SiO2, toluene/methylene chloride/ethyl acetate 10:10:3)