反应详情

To a dry THF solution (20 mL) of methyl N-(4-bromo-5-methylisoxazol-3-yl)-N-[(2,2,2-trichloroethoxy)carbonyl]leucinate (1.19 g, 2.47 mmol) and activated zinc (10.1 g, 154 mmol) was added ca. 10 mL of 1 M KH2PO4 (10 mmol) at 0° C. The mixture was stirred for 1.5 hours, filtered through celite, washed with 150 mL ethyl acetate, and concentrated to a small volume. The mixture was then partitioned between ethyl acetate and saturated aqueous sodium bicarbonate, washed with brine, dried over sodium sulphate and concentrated in vacuo. The crude product was purified by flash chromatography (20% ethyl acetate/hexane) to afford methyl N-(4-bromo-5-methylisoxazol-3-yl)leucinate.

1. filtrationfiltered through celite
2. washwashed with 150 mL ethyl acetate
3. concentrationconcentrated to a small volume
4. customThe mixture was then partitioned between ethyl acetate and saturated aqueous sodium bicarbonate
5. washwashed with brine
6. dry with materialdried over sodium sulphate
7. concentrationconcentrated in vacuo
8. customThe crude product was purified by flash chromatography (20% ethyl acetate/hexane)