反应详情

To a suspension of 7.24 g of (2-bromo-4-fluorophenyl)hydrazine hydrochloric acid salt in 100 mL of acetic acid, 5.5 g of ethyl 2-(2-oxocyclohexyl)-acetate was added. The resulting mixture was heated to reflux for 1 h. Then 10 mL of ethanol was added and the reaction mixture was heated at reflux overnight. The solvent was evaporated and the residue was diluted with EtOAc and washed with saturated aqueous NaHCO3 solution, water, and brine successively. The organic layer was separated and dried over anhydrous sodium sulfate, filtered, and evaporated. The residue was purified by flash chromatography over silica gel (5% EtOAc/hexane) to afford 3.12 g of desired compound.

1. additionwas added
2. temperatureThe resulting mixture was heated
3. temperatureto reflux for 1 h
4. temperaturethe reaction mixture was heated
5. temperatureat reflux overnight
6. customThe solvent was evaporated
7. additionthe residue was diluted with EtOAc
8. washwashed with saturated aqueous NaHCO3 solution, water, and brine successively
9. customThe organic layer was separated
10. dry with materialdried over anhydrous sodium sulfate
11. filtrationfiltered
12. customevaporated
13. customThe residue was purified by flash chromatography over silica gel (5% EtOAc/hexane)