反应详情

A solution of compound 110 (236 mg, 0.46 mmol) in MeOH (3.0 mL) was added LiOH (55 mg, 2.31 mmol) and water (0.3 mL). The reaction mixture was stirred for 2 h under reflux. The reaction mixture was poured into a mixture of EtOAc/saturated NaCl. Aq. HCl (1 N, 0.5 mL) was added. The aqueous phase was washed with more EtOAc. The collected organic phases were washed with water, brine and then dried (MgSO4), filtered and concentrated in vacuo to give the crude product. The crude product was purified by flash chromatography using a mixture of MeOH/DCM/acetic acid 400:2:1 as the eluent to afford the title compound as yellow foam. 13C NMR (DMSO-d6) δ 194.9, 168.4, 158.7 (dd), 155.7 (dd), 149.3, 145.3, 139.8, 136.0, 133.7, 133.7, 131.7, 128.1, 127.1, 126.5, 126.4 (dd), 125.0, 124.2 (dd), 122.8, 114.8, 112.0 (dd), 111.8, 105.0 (dd), 50.9, 19.4

1. temperatureunder reflux
2. washThe aqueous phase was washed with more EtOAc
3. washThe collected organic phases were washed with water, brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customto give the crude product
8. customThe crude product was purified by flash chromatography
9. additiona mixture of MeOH/DCM/acetic acid 400:2:1 as the eluent