反应详情

温度

20 °C

Triethylamine (0.09 ml) was added to solution of Intermediate 3 (0.150 g, 0.545 mmol) in dichloromethane (3 ml) with stirring at 20° C. under nitrogen. The solution was cooled to 0° C. and a solution of 4-nitrophenyl chloroformate (0.121 g) in dichloromethane (1 ml) was added drop-wise. The resultant mixture was stirred for 4 h at 0° C. The solution was allowed to warm to 20° C., washed with brine (4 ml), dried (MgSO4), and concentrated in vacuo. Purification by Biotage flash chromatography on silica gel, eluting with 35% ethyl acetate in cyclohexane, gave the title compound as a pale yellow solid (0.119 g). LC/MS (system A) Rt 3.01 min, Mass Spectrum m/z 441 [MH+].

1. temperatureThe solution was cooled to 0° C.
2. temperatureto warm to 20° C.
3. washwashed with brine (4 ml)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customPurification by Biotage flash chromatography on silica gel
7. washeluting with 35% ethyl acetate in cyclohexane