反应详情

To a solution of ester from Step 5 (3.5 g, 7.6 mmol) in MeOH/THF (50 mL/35 mL) was added 1M NaOH (22.9 mL, 22.9 mmol). After heating at reflux for 2 h, the mixture was concentrated under vacuum and the residue was partitioned between EtOAc/H2O containing HOAc (3 mL). The organic layer was washed with H2O, brine, and was then dried (MgSO4), filtered, and evaporated. The resulting solid was stirred vigorously with 1:10 EtOAc/hexane for 2 h to give, after filtration, 2.81 g of white solid.

1. temperatureAfter heating
2. temperatureat reflux for 2 h
3. concentrationthe mixture was concentrated under vacuum
4. customthe residue was partitioned between EtOAc/H2O
5. additioncontaining HOAc (3 mL)
6. washThe organic layer was washed with H2O, brine
7. dry with materialwas then dried (MgSO4)
8. filtrationfiltered
9. customevaporated
10. customto give
11. filtrationafter filtration, 2.81 g of white solid