反应详情

To a solution of 1.245 g (4.151 mmol) 6-amino-1-hydroxy-3,3-bis-trifluoromethyl-1,3-dihydro-indol-2-one in 80 ml THF was added 3.565 ml (62.27 mmol) glacial AcOH and 19 g (290.6 mmol) Zinc dust (100 mesh). The reaction was stirred 40 min at RT and then 5 h at reflux. The reaction was cooled to RT. The solvent was decanted and concentrated, then dissolved in EtOAc and filtered through Celite®. The EtOAc solution was then washed with saturated aqueous NaHCO3 and brine, dried over Na2SO4, filtered, and concentrated and dried under vacuum, to yield the titled compound, as a yellow solid.

1. temperature5 h at reflux
2. temperatureThe reaction was cooled to RT
3. customThe solvent was decanted
4. concentrationconcentrated
5. dissolutiondissolved in EtOAc
6. filtrationfiltered through Celite®
7. washThe EtOAc solution was then washed with saturated aqueous NaHCO3 and brine
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated
11. customdried under vacuum