反应详情

(1R)-1-[5-(3-chlorophenyl)isoxazol-3-yl]ethyl acetate (56 g, 211 mmol) and lithium hydroxide monohydrate (10.6 g, 253 mmol) were mixed with THF/Water (7/5, 1.2 L) and stirred at r.t. over night. Reducing the volume of the mixture in vacuo to about ½, followed by dilution with brine, extraction with ether and then drying over MgSO4 and in vacuo concentration gave crude product. The crude product was purified by flash column chromatography on silica using heptane/EtOAc=70:30, to give the title compound (40 g, 85%). 1H NMR: 7.73 (m, 1H), 7.63 (m, 1H), 7.38 (m, 2H), 6.57 (s, 1H), 5.07 (q, 1H), 2.44 (s, 1H), 1.59 (d, 3H).

1. extractionfollowed by dilution with brine, extraction with ether
2. dry with materialdrying over MgSO4 and in vacuo concentration
3. customgave crude product
4. customThe crude product was purified by flash column chromatography on silica