反应详情

温度

80 °C

A mixture of (5)-tert-butyl 2-(4-aminophenyl)morpholine-4-carboxylate (100 mg, 0.36 mmol), 2,4,5-trichloropyrimidine (66 mg, 0.36 mmol) and diisopropylethylamine (70 mg, 0.54 mmol) was dissolved in 2-propanol (1.5 ml) and stirred at 80° C. overnight. For work-up most of the solvent was evaporated, then aqueous ammonium chloride solution was added and the mixture was extracted with ethyl acetate. The aqueous phase was re-extracted with ethyl acetate twice. The combined organic layers were dried (MgSO4) and concentrated in vacuo. The residue was purified by flash chromatography (20 g silica gel, 10 to 30% ethyl acetate in heptane) to yield a white solid (141 mg, 92%). MS (ISP): 425.1 ([{35Cl}M+H]+), 427.1 ([{37Cl}M+H]+).

1. customFor work-up most of the solvent was evaporated
2. additionaqueous ammonium chloride solution was added
3. extractionthe mixture was extracted with ethyl acetate
4. extractionThe aqueous phase was re-extracted with ethyl acetate twice
5. dry with materialThe combined organic layers were dried (MgSO4)
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography (20 g silica gel, 10 to 30% ethyl acetate in heptane)