反应详情

Dissolve 1,1-dimethylethyl(4R)-3-oxo-4-[({[(phenylmethyl)oxy]carbonyl}amino)methyl]-1-pyrrolidinecarboxylate (0.87 g, 2.49 mmol) in 5:1 MeOH/H O (10 mL). Add in hydroxylamine HCl (0.177 g, 2.54 mmol) and sodium acetate (2.04 g, 24.9 mmol). The mixture was heated to reflux and allowed to stir 3 hours. After the reaction was complete the solution was concentrated under reduced pressure and extracted with CHCl3 (3×). The organic layer was washed with 0.5 M HCl and brine. The solution was dried over Na2SO4, and evaporated to yield an oil. (0.90 g, quant). LCMS: m/z 364.6 (MH+).

1. temperatureThe mixture was heated
2. temperatureto reflux
3. concentrationwas concentrated under reduced pressure
4. extractionextracted with CHCl3 (3×)
5. washThe organic layer was washed with 0.5 M HCl and brine
6. dry with materialThe solution was dried over Na2SO4
7. customevaporated
8. customto yield an oil