反应详情

In a sealed tube, 780 mg (6 m mole) of 5-fluorouracil, 5 ml of pyridine, 100 mg (0.44 m mole) of antimony trichloride and 1.26 g (18 m mole) of 2,3-dihydrofuran were heated at 100° C for 3 hours. The reaction mixture was further admixed with 800 mg (11.5 m mole) of 2,3-dihydrofuran and the mixture was heated for 17 hours. After the reaction, pyridine was distilled off under a reduced pressure and the residue was dissolved in chloroform and the insoluble matters were separated by a filtration. Chloroform was distilled off from the filtrate and the residue was purified by a column chromatography using a silica gel column (mixture of chloroform and acetone = 8 : 1 (V/V) as a developing medium) to obtain 1.10 g of N1,N3 -bis(2-tetrahydrofuryl)-5-fluorouracil (yield: 68.0%) and 325 mg of N1 -(2-tetrahydrofuryl)-5-fluorouracil (yield: 27%).

1. temperaturethe mixture was heated for 17 hours
2. distillationwas distilled off under a reduced pressure
3. dissolutionthe residue was dissolved in chloroform
4. customthe insoluble matters were separated by a filtration
5. distillationChloroform was distilled off from the filtrate
6. customthe residue was purified by a column chromatography
7. additionmixture of chloroform and acetone = 8 : 1 (V/V) as a developing medium)