HRID1413194
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In a closed tubular reactor, 1.3 g of 5-fluorouracil, 5 ml of benzene and 14 g of 2,3-dihydrofuran were heated together at 200° C. for 6 hours. After cooling, the reaction mixture was concentrated to dryness under reduced pressure and the residue was separated and purified by column chromatography on 25 g silica gel. From the chloroform eluate, the fractions rich in the contemplated compound were collected. The solvent was distilled off and the residue was recrystallized from petroleum ether. By the above procedure was obtained 1.3 g of 1,3-bis-(tetrahydro-2-furyl)-5-fluorouracil.
WORKUP
后处理
- temperatureAfter cooling
- concentrationthe reaction mixture was concentrated to dryness under reduced pressure
- customthe residue was separated
- custompurified by column chromatography on 25 g silica gel
- customFrom the chloroform eluate, the fractions rich in the contemplated compound were collected
- distillationThe solvent was distilled off
- customthe residue was recrystallized from petroleum ether