反应详情

A mixture of 2 (1.3 g, 4.07 mmol), 2N NaOH (12 mL), and MeOH (62 mL) was refluxed for 40 h. The organic solvent was evaporated and the remaining residue was extracted with EtOAc. The combined extract were washed with brine, dried (Na2SO4) and evaporated in vacuo to give a residue which was purified by flash chromatography (silica gel, cyclohexane/ethyl acetate, 8:2) and crystallization from ether/cyclohexane.

1. temperaturewas refluxed for 40 h
2. customThe organic solvent was evaporated
3. extractionthe remaining residue was extracted with EtOAc
4. extractionThe combined extract
5. washwere washed with brine
6. dry with materialdried (Na2SO4)
7. customevaporated in vacuo
8. customto give a residue which
9. customwas purified by flash chromatography (silica gel, cyclohexane/ethyl acetate, 8:2) and crystallization from ether/cyclohexane