反应详情

温度

85 °C

(E)-Methyl 5-(2-ethoxyvinyl)-2-(methylthio)pyrimidine-4-carboxylate (Preparation 31, 2.30 g, 9.04 mmol) was treated with ammonia in methanol 7M (45 mL) and heated to 85° C. for 18 hours in a capped vial. The solvent was removed under reduced pressure, and the resulting solid was treated with TsOH monohydrate (175 mg, 0.92 mmol), suspended in toluene (50 mL) and heated to 90° C. for 2 hours. The mixture was concentrated and the residue was purified by silica gel column chromatography eluting with 0 to 5% MeOH in DCM to give the title compound (1.47 g, 84%).

1. customThe solvent was removed under reduced pressure
2. temperatureheated to 90° C. for 2 hours
3. concentrationThe mixture was concentrated
4. customthe residue was purified by silica gel column chromatography
5. washeluting with 0 to 5% MeOH in DCM