反应详情

In 10 ml of pyridine were dissolved 2.9 g (10 mmol) of isobutyl 5-fluoro-6-acetoxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate and 2.22 g (20 mmol) of (E)-furfuraldoxime, and 1.01 g (10 mmol) of dried triethylamine was added to the solution, followed by stirring at room temperature for 21 hours. The reaction solution was concentrated under reduced pressure, and 50 ml of ethyl acetate was added to the residue. The organic layer was washed three times with 10-ml portions of water, and the solvent was dried and evaporated under reduced pressure. The residue was recrystallized twice from ethyl acetate-hexane to give 2.39 g of isobutyl 5-fluoro-6-(E)-furfurylideneaminooxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate. m.p. 167°-168° C.

1. additionwas added to the solution
2. concentrationThe reaction solution was concentrated under reduced pressure, and 50 ml of ethyl acetate
3. additionwas added to the residue
4. washThe organic layer was washed three times with 10-ml portions of water
5. customthe solvent was dried
6. customevaporated under reduced pressure
7. customThe residue was recrystallized twice from ethyl acetate-hexane