反应详情

To a stirred solution of ethyl 2-(acetonylamino)-2-oxo-acetate (9.2 g, 53.12 mmol) in toluene (100.0 mL), is added POCl3 (4.95 mL, 53.12 mmol) and the reaction mixture is refluxed for 16 hours. The reaction mixture is cooled, added portionwise to water (100.0 mL) and stirred vigorously. The organic layer is washed with saturated NaHCO3 solution (2×50 mL), water (2×50 mL), dried over Na2SO4, and evaporated under reduced pressure. The crude material is purified by silica gel chromatography eluting with hexane:ethyl acetate (8.0:2.0) to give the title compound (5.1 g, 61.9%) as a yellow oil. ESI/MS m/z 156.2.1 (M+H)+.

1. temperaturethe reaction mixture is refluxed for 16 hours
2. temperatureThe reaction mixture is cooled
3. washThe organic layer is washed with saturated NaHCO3 solution (2×50 mL), water (2×50 mL)
4. dry with materialdried over Na2SO4
5. customevaporated under reduced pressure
6. customThe crude material is purified by silica gel chromatography
7. washeluting with hexane:ethyl acetate (8.0:2.0)