反应详情

温度

80 °C

To a solution of 8-chloro-2-(methylthio)pyrido[3,4-d]pyrimidine (Preparation 33, 1 g, 4.72 mmol) in NMP (15 mL) was added neopentylamine (5.5 mL, 4.72 mmol). The reaction mixture was heated to 80° C. for 20 hours. The reaction mixture was diluted with saturated aqueous NaHCO3 (50 mL) and EtOAc (2×50 mL). The combined organic layers were washed with water (50 mL) and brine (50 mL), dried (MgSO4) and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with 0-100% EtOAc in cyclohexane give the title compound (915 mg, 74%).

1. washThe combined organic layers were washed with water (50 mL) and brine (50 mL)
2. dry with materialdried (MgSO4)
3. concentrationconcentrated in vacuo
4. customThe residue was purified by silica gel column chromatography
5. washeluting with 0-100% EtOAc in cyclohexane