反应详情

温度

70 °C

2.6 g (0.02 mole) of 5-fluorouracil was suspended in 10 ml of absolute pyridine, and the suspension was stirred at 70° C to form a solution. 17 g (0.12 mole) of benzoyl chloride was added dropwise to the resulting solution followed by heating to 80° C for 1.5 hours while stirring. After completion of the reaction, the reaction mixture was concentrated under reduced pressure (25 mm Hg) to half its original volume, and 50 ml of ethyl acetate was added thereto. After the insoluble matter in the ethyl acetate was removed, the solution was washed twice with water, and dried over Glauber's salt, and the ethyl acetate removed therefrom under reduced pressure (25 mm Hg). Ethanol was then added to the residue, and the mixture heated to 80° C to form a solution followed by allowing the resulting solution to cool to precipitate crystals, which were then filtered to obtain 3.4 g of 1,3-di-N-benzoyl-5-fluorouracil in a yield of 51%.

1. customto form a solution
2. temperatureby heating to 80° C for 1.5 hours
3. stirringwhile stirring
4. customAfter completion of the reaction
5. concentrationthe reaction mixture was concentrated under reduced pressure (25 mm Hg) to half its original volume, and 50 ml of ethyl acetate
6. additionwas added
7. customAfter the insoluble matter in the ethyl acetate was removed
8. washthe solution was washed twice with water
9. dry with materialdried over Glauber's salt
10. customthe ethyl acetate removed
11. additionEthanol was then added to the residue
12. temperaturethe mixture heated to 80° C
13. customto form a solution
14. temperatureto cool
15. customto precipitate crystals, which
16. filtrationwere then filtered