HRID373242

反应详情

EQUATION

反应方程式

HRID 373242 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 3-butyl-6-chloropyrimidine-2,4(1H,3H)-dione (1 g), 4-bromomethyl-2'-(N-trityltetrazol-5-yl)biphenyl (3.02 g) and potassium carbonate (0.82 g) in DMF (50 ml) was stirred at 60° C. for 4 hours. The reaction mixture was concentrated to dryness in vacuo and then the residue was dissolved in methylene chloride. The insoluble material was removed from the reaction mixture by filtration and the filtrate was concentrated to dryness. The resulting residue was purified by column chromatography on silica gel and recrystallized from ethyl acetate-hexane to give colorless prisms (1.97 g, 59%).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated to dryness in vacuo
  2. dissolutionthe residue was dissolved in methylene chloride
  3. customThe insoluble material was removed from the reaction mixture by filtration
  4. concentrationthe filtrate was concentrated to dryness
  5. customThe resulting residue was purified by column chromatography on silica gel
  6. customrecrystallized from ethyl acetate-hexane