反应详情

温度

60 °C

In 45 ml of pyridine-acetone (pyridine:acetone=2:1) were dissolved 11.6 g (40 mmol) of isobutyl 5-fluoro-6-acetoxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate and 6.1 g (54.9 mmol) of (Z)-furfuraldoxime, and the solution was stirred at 60° C. for 16 hours. The solvent was distilled off under reduced pressure, and the residue was dissolved in 150 ml of ethyl acetate. The solution was washed three times with 50-ml portions of water, and the ethyl acetate layer was dried and the solvent was evaporated under reduced pressure. The residue was recrystallized three times from ethyl acetate-hexane to give 5.5 g of isobutyl 5-fluoro-6-(Z)-furfurylideneaminooxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate. m.p. 159°-160° C.

1. distillationThe solvent was distilled off under reduced pressure
2. dissolutionthe residue was dissolved in 150 ml of ethyl acetate
3. washThe solution was washed three times with 50-ml portions of water
4. dry with materialthe ethyl acetate layer was dried
5. customthe solvent was evaporated under reduced pressure
6. customThe residue was recrystallized three times from ethyl acetate-hexane