HRID1112268

反应详情

EQUATION

反应方程式

HRID 1112268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a sealed tube, 780 mg (6 m mole) of 5-fluorouracil, 5 ml of pyridine, 100 mg (0.70 m mole) of phosphorus pentoxide and 1.26 g (18 m mole) of 2,3-dihydrofuran were heated at 100° C for 17 hours. After the reaction, pyridine was distilled off from the reaction mixture under a reduced pressure. The residue was dissolved in chloroform and the insoluble unreacted 5-fluorouracil was separated by a filtration and the residue was purified by a column chromatography using a silica gel column (mixture of benzene; ethyl acetate and acetone = 2 : 1 : 1 (V/V) as a developing medium) to obtained 200 mg of N1,N3 -bis(2-tetrahydrofuryl)-5-fluorouracil (yield: 12.3%) and 757.6 mg of N1 -(2-tetrahydrofuryl)-5-fluorouracil (yield: 63.0%).

WORKUP

后处理

  1. distillationwas distilled off from the reaction mixture under a reduced pressure
  2. dissolutionThe residue was dissolved in chloroform
  3. customthe insoluble unreacted 5-fluorouracil was separated by a filtration
  4. customthe residue was purified by a column chromatography
  5. additionmixture of benzene