反应详情

A solution was made containing (2S)-1-(tert-butoxycarbonyl)-4-oxo-2-pyrrolidinecarboxylic acid (5.0 g, 22 mmol) and O-allylhydroxylamine hydrochloride monohydrate (7.2 g, 65.5 mmol) in a 1:1 mixture of pyridine and ethanol (100 ml). The reaction was heated to reflux for 2.5 h before cooling and removal of solvent. The residue was dissolved in ethyl acetate and washed rapidly with 1.3N HCl (40 ml). The acidic layer was then extracted with ethyl acetate (3×20 ml) and the combined organic layers washed with brine before drying over magnesium sulfate, filtering and removal of solvent in vacuo. The desired product (5.9 g, 94%) was isolated as a pale yellow oil.

1. temperatureThe reaction was heated
2. temperatureto reflux for 2.5 h
3. temperaturebefore cooling
4. customremoval of solvent
5. dissolutionThe residue was dissolved in ethyl acetate
6. washwashed rapidly with 1.3N HCl (40 ml)
7. extractionThe acidic layer was then extracted with ethyl acetate (3×20 ml)
8. washthe combined organic layers washed with brine
9. dry with materialbefore drying over magnesium sulfate
10. filtrationfiltering
11. customremoval of solvent in vacuo