反应详情

温度

105 °C

The mixture of N-(3,3-dimethyl-2-oxo-butyl)-oxalamic acid ethyl ester (0.79 g, 3.67 mmol) and phosphorus oxychloride (2.0 mL, 22.0 mmol) was stirred at 105° C. under N2 for 2 h, cooled to RT, quenched slowly with ice-water, extracted with EtOAc. The combined organic portions were washed with brine, dried with Na2SO4, removal of the solvents gave a dark brownish oil which was purified by flash column chromatography to yield the title compound. MS m/z: 197.9 (M+H). Calc'd for C10H15NO3-197.23

1. temperaturecooled to RT
2. customquenched slowly with ice-water
3. extractionextracted with EtOAc
4. washThe combined organic portions were washed with brine
5. dry with materialdried with Na2SO4, removal of the solvents
6. customgave a dark brownish oil which
7. customwas purified by flash column chromatography