反应详情

温度

100 °C

5-Benzoyl-6-(bromomethyl)-1,3-dimethylpyrimidine-2,4(1H,3H)-dione (Intermediate A step 3) (400 mg 1.19 mmol) in EtOH (4 mL) was treated with TEA (0.16 mL, 1.19 mmol) and ethanolamine (72.5 mg, 1.19 mmol). The mixture was heated to 100° C. for 1 h under microwave irradiation. A further portion of ethanolamine (96 μL) was added and heating continued for a further 20 min. The reaction was poured into DCM (75 mL) and water (75 mL). The layers were separated and the aqueous phase extracted with DCM (2×50 mL). The combined organic phases were washed with water (2×50 mL), then passed through a hydrophobic frit. The solvent was removed under reduced pressure affording a pale yellow solid. The solid was triturated in hot EtOH and allowed to cool. The title product was collected by reduced pressure filtration as a white powder.

1. temperatureheating
2. customThe layers were separated
3. extractionthe aqueous phase extracted with DCM (2×50 mL)
4. washThe combined organic phases were washed with water (2×50 mL)
5. customThe solvent was removed under reduced pressure
6. customaffording a pale yellow solid
7. customThe solid was triturated in hot EtOH
8. temperatureto cool
9. filtrationThe title product was collected by reduced pressure filtration as a white powder