反应详情

温度

0 °C

A solution of (2-cyano-1-ethyl-2-hydroxy-ethyl)-carbamic acid tert-butyl ester (9.53 g, 44 mmol) in methanol (80 ml) was cooled to 0° C. and treated successively with hydroxylamine hydrochloride (3.05, 44 mmol) in methanol (80 ml) and 25% sodium methoxide solution in methanol (10.2 ml). Stirred at 0° C. for 5 minutes, cold bath removed and the reaction mixture stirred at room temperature for 5 hours. Methanol evaporated off under reduced pressure, crude partitioned between ethyl acetate and water. Organic layer separated, dried (MgSO4) and evaporated under reduced pressure to give yellow oil. Purified by mplc, eluting with a mixture of ethyl acetate-heptane to give the title compound as white solid (3.5 g); MS: M(H+) 248.

1. customcold bath removed
2. stirringthe reaction mixture stirred at room temperature for 5 hours
3. customMethanol evaporated off under reduced pressure, crude
4. custompartitioned between ethyl acetate and water
5. customOrganic layer separated
6. dry with materialdried (MgSO4)
7. customevaporated under reduced pressure
8. customto give yellow oil
9. customPurified by mplc
10. washeluting with a mixture of ethyl acetate-heptane