反应详情

A solution of 5.0 g of 1-acetyl-4-(2,4-difluorobenzoyl)piperidine, 1.2 g of methylhydrazine and 50 ml of n-butanol was heated under reflux for 16 hrs. After cooling, the solvent was removed in vacuo and the residue was diluted with water. The aqueous mixture was made basic with ammonium hydroxide and extracted with dichloromethane. The organic extract was washed with water, dried over anhydrous magnesium sulfate and concentrated to yield 5.6 g of 3-(1-acetyl-4-piperidinyl)-6-fluoro-1-methyl-1H-indazole as an oil.

1. temperatureunder reflux for 16 hrs
2. temperatureAfter cooling
3. customthe solvent was removed in vacuo
4. additionthe residue was diluted with water
5. extractionextracted with dichloromethane
6. extractionThe organic extract
7. washwas washed with water
8. dry with materialdried over anhydrous magnesium sulfate
9. concentrationconcentrated