反应详情

Methanesulfonyl chloride (887 μl, 7.20 mmol) was added to a suspension of 5-nitroindazole (979 mg, 6.00 mmol) and triethylamine (2.0 ml, 14.3 mmol) in dichloromethane (20 ml) at 0° C., and the resulting mixture was stirred at room temperature for 3 hours. Methanesulfonyl chloride (222 μl, 1.80 mmol) was further added thereto, followed by stirring for another 1 hour. The reaction mixture was poured into a saturated aqueous sodium hydrogencarbonate solution to terminate the reaction, followed by extraction with chloroform. The extract solution was washed with a saturated aqueous sodium chloride solution, dried over sodium sulfate, and then distilled under reduced pressure to remove the solvent. The residue was purified by washing with methanol to obtain 1-(methylsulfonyl)-5-nitro-1H-indazole (1.16 g, 80%).

1. stirringby stirring for another 1 hour
2. customto terminate
3. customthe reaction
4. extractionfollowed by extraction with chloroform
5. washThe extract solution was washed with a saturated aqueous sodium chloride solution
6. dry with materialdried over sodium sulfate
7. distillationdistilled under reduced pressure
8. customto remove the solvent
9. customThe residue was purified
10. washby washing with methanol