HRID29189
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
tert-Butyl-N-((1S)-1-[(2S)oxiranyl]-2-phenylethylcarbamate (0.155 g, 0.59 mmol) and O-(tert-butyl)hydroxylamine hydrochloride (0.089 g, 0.71 mmol) were heated with diisopropylethylamine (0.154 ml, 0.88 mmol) in isopropanol (2 ml) in a sealed tube at 60° C. for 5 days. The reaction mixture was concentrated in vacuo, taken up in EtOAc, washed with sat. aq. NaHCO3, and brine. The organic phase was dried over MgSO4, filtered and solvent removed in vacuo. Purication by column chromatography (1% MeOH in CH2Cl2) gave 100 mg of a white solid which was used directly in the next reaction.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- washwashed with sat. aq. NaHCO3, and brine
- dry with materialThe organic phase was dried over MgSO4
- filtrationfiltered
- customsolvent removed in vacuo