HRID2372518

反应详情

EQUATION

反应方程式

HRID 2372518 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 2'-deoxyuridine (100 g, 0.44 mol) and triphenylmethyl choride (147 g, 0.53 mol) in 250 mL of pyridine was heated at 100° C. for 30 minutes. One-third of the cooled solution was added at a slow flow rate to a mixture of ice water (2:3) in a commercial blender blending for 3-5 minutes after adding the solution. The resulting white precipitate was filtered and washed twice, stirring in 2 L of water. Recrystallization was accomplished by refluxing the product in a benzene-acetone solution (1:1) for 15 minutes, yielding 128 g (62%). The compound softened at 76° C., began to melt at 152-155° C., and darkened in color at 155-159° C. Rf =0.71 (CHCl3 --EtOH, 4:1).

WORKUP

后处理

  1. additionafter adding the solution
  2. filtrationThe resulting white precipitate was filtered
  3. washwashed twice
  4. customRecrystallization
  5. temperatureby refluxing the product in a benzene-acetone solution (1:1) for 15 minutes
  6. customyielding 128 g (62%)
  7. customsoftened at 76° C.
  8. customto melt at 152-155° C.
  9. customdarkened in color at 155-159° C