反应详情

温度

60 °C

A suspension of intermediate 33, ethyl 2-(2-(3-chloropropoxy)propan-2-yl)-5-hydroxy-6-oxo-1,6-dihydropyrimidine-4-carboxylate, (0.205 g, 0.64 mmol) and anhydrous potassium carbonate (0.361 g, 2.6 mmol) in anhydrous dimethylformamide (4 mL) was stirred at 60° C. for 5 hours. The reaction mixture was treated with benzyl bromide (0.122 g, 0.71 mmol) and stirred for 16 hours. Following this, 2 mL of H2O was added and the mixture stirred for an additional 24 hours. Solvent was removed by rotary evaporator and the resulting residue suspended in 0.5 N hydrochloric acid (16 mL). The crude product was extracted with ethyl acetate (2×15 mL), then dried (sodium sulfate), filtered, and concentrated to dryness by rotary evaporator to give 0.299 g (Yield >100%) of the title compound as a solid. LC/MS [M+H]+=345.21.

1. stirringstirred for 16 hours
2. additionwas added
3. stirringthe mixture stirred for an additional 24 hours
4. customSolvent was removed by rotary evaporator
5. extractionThe crude product was extracted with ethyl acetate (2×15 mL)
6. dry with materialdried (sodium sulfate)
7. filtrationfiltered
8. concentrationconcentrated to dryness by rotary evaporator