反应详情

The solution of (5) (2.4 g, 0.009 mol) in methyl alcohol (25 ml) was added with 1N NaOH (13.5 ml) and the mixture was left under stirring for 8 hours at room temperature. After evaporating the solvent, the residue was diluted with water and 5% monobasic sodium phosphate was added drop by drop to the mixture to adjust pH to 5. The aqueous layer was then extracted with methyl acetate (2×100 ml). The collected organic extracts were dried over Na2SO4 and evaporated under vacuum, then crystallized from a benzene/petroleum ether 6:20 mixture to obtain 2.05 g of (6) (0.0081 mol; yield 90%) as a white solid (melting point 92-92° C.) following crystallization.

1. waitthe mixture was left
2. customAfter evaporating the solvent
3. additionthe residue was diluted with water and 5% monobasic sodium phosphate
4. additionwas added drop by drop to the mixture
5. extractionThe aqueous layer was then extracted with methyl acetate (2×100 ml)
6. dry with materialThe collected organic extracts were dried over Na2SO4
7. customevaporated under vacuum
8. customcrystallized from a benzene/petroleum ether 6:20 mixture