反应详情

To a solution of Compound 1e (0.18 g, 0.86 mmol) in THF (8 mL) was added 1 M LiOH (2.6 mL, 2.6 mmol) at rt. After 5 h, the organic solvent was evaporated under reduced pressure and the resultant aqueous layer was diluted with water and acidified by the addition of 1 N HCl solution to pH ˜2. The solution was extracted with EtOAc (2×) and the combined extracts were dried (Na2SO4), filtered and concentrated under reduced pressure to afford Compound 1a (150 mg, 92%) as a white solid. LCMS=0.67 min using analytical method (B), 189.9 (M+H). 1H NMR (400 MHz, CD3OD) δ 3.15-2.89 (m, 2H), 1.72 (s, 3H).

1. customthe organic solvent was evaporated under reduced pressure
2. additionthe resultant aqueous layer was diluted with water
3. additionacidified by the addition of 1 N HCl solution to pH ˜2
4. extractionThe solution was extracted with EtOAc (2×)
5. dry with materialthe combined extracts were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure