HRID1649118

反应详情

EQUATION

反应方程式

HRID 1649118 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Bis(trimethylsilyl)-5-fluorouracil prepared from 5-fluorouracil (10 g), and 2-2,6-dichlorophenyl-1,3-dioxolan (32.0 g) which had been prepared from 2,6-dichlorobenzaldehyde and ethylene glycol were subjected to reaction as in Example 10. Following adding chloroform (100 ml), the reaction mixture was washed twice with a cold saturated NaCl aqueous solution, and then aqueous sodium bicarbonate, and water, and dried over anhydrous magnesium sulfate. The solvent was evaporated off and the residue was purified by column chromatography using silica gel and acetone-chloroform (1:4) as an eluant to give 6.9 g of crystalline 1-[α-(2-hydroxyethoxy)-2,6-dichlorobenzyl]-5-fluorouracil.

WORKUP

后处理

  1. customwere subjected to reaction as in Example 10
  2. washthe reaction mixture was washed twice with a cold saturated NaCl aqueous solution
  3. dry with materialaqueous sodium bicarbonate, and water, and dried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated off
  5. customthe residue was purified by column chromatography