反应详情

温度

0 °C

A solution of LiAlH4 (213 mg, 5.62 mmol) in anhydrous THF (8 mL) was added slowly to a solution of ethyl 2-(t-butoxycarbonylaminooxy)propanoate (820 mg, 3.52 mmol) in THF (15 mL) at 0° C. The mixture was stirred at 0° C. for 5 h and then at rt overnight. The solution was quenched with a mixture of Na2SO4 and water, and stirred for an additional 1.5 h. The mixture was filtered and concentrated. The crude was dissolved in EtOAc, washed with water and brine, and then dried over Na2SO4. Solvent was evaporated to afford the title compound as a clear oil (500 mg, 74.4%). 1H-NMR (400 MHz, CDCl3) δ ppm 7.09 (s, 1H), 3.95 (m, 1H), 3.69 (dd, 1H), 3.47 (m, 1H), 1.51 (s, 9H), 1.21 (d, 3H).

1. customat rt
2. customovernight
3. customThe solution was quenched with a mixture of Na2SO4 and water
4. stirringstirred for an additional 1.5 h
5. filtrationThe mixture was filtered
6. concentrationconcentrated
7. dissolutionThe crude was dissolved in EtOAc
8. washwashed with water and brine
9. dry with materialdried over Na2SO4
10. customSolvent was evaporated