反应详情

A mixture of 1-(5-bromo-2-hydroxy-phenyl)-ethanone (20 g, 0.093 mol), 4-methylcyclohexanone (21.31 g, 0.187 mol) and pyrrolidine (12.63 g, 0.178 mol) in methanol (400 mL) was refluxed for overnight. The reaction mixture was concentrated in vacuo, diluted with an equal volume of H2O and then added HCl until pH=1. The resulting mixture was extracted with EtOAc. The organic layer was dried over anhydrous Na2SO4, filtered, and evaporated to give 6-bromo-4′-methylspiro(chroman-2,1′-cyclohexan)-4-one (45 g, 100%).

1. temperaturewas refluxed for overnight
2. concentrationThe reaction mixture was concentrated in vacuo
3. additiondiluted with an equal volume of H2O
4. extractionThe resulting mixture was extracted with EtOAc
5. dry with materialThe organic layer was dried over anhydrous Na2SO4
6. filtrationfiltered
7. customevaporated