反应详情

2-Hydrazino-5-(methylsulfonyl)pyridine hydrochloride (448 mg, 2 mmol) and TFA (1.38 mL, 18 mmol) were mixed in trifluoroethanol (10 mL) and stirred for 5 minutes 4,4-Difluoro-1-cyclohexyl-1,3-butanedione (408 mg, 2 mmol) was added. The resulting reaction mixture was heated at reflux temperature for 60 hours. The solvent was then removed in vacuo, and the residue was partitioned between EtOAc and water. The organic layer was washed with brine and concentrated in vacuo. The product was purified by recrystallization from 3:1 of isooctane:methylene chloride to give the title compound (346 mg, 49%).

1. additionwas added
2. customThe resulting reaction mixture
3. temperaturewas heated
4. temperatureat reflux temperature for 60 hours
5. customThe solvent was then removed in vacuo
6. customthe residue was partitioned between EtOAc and water
7. washThe organic layer was washed with brine
8. concentrationconcentrated in vacuo
9. customThe product was purified by recrystallization from 3:1 of isooctane