反应详情

To a suspension of 700 mg (3.66 mmol) of 6-amino-5-methyl-1H-indazole-7-carboxylic acid in 26 mL of anhydrous acetonitrile is added 1.11 g (3.66 mmol) of 5-bromo-2-(3-chloro-pyridin-2-yl)-2H-pyrazole-3-carboxylic acid followed by 1.3 mL (16.2 mmol) of pyridine. The mixture is stirred at ambient temperature during 30 minutes. Then the suspension is cooled to 0° C. and 1.0 mL (12.9 mmol) of methanesulfonyl chloride is added drop wise. The mixture is stirred at ambient temperature for 16 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. The pale yellowish product obtained (1.6 g) is engaged in the next step; LC/MS:459/461 (M+H)+.

1. temperatureThen the suspension is cooled to 0° C.
2. stirringThe mixture is stirred at ambient temperature for 16 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. customThe pale yellowish product obtained (1.6 g)