HRID879953

反应详情

EQUATION

反应方程式

HRID 879953 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

AICA riboside (1.00 g), triphenylphosphine (3.05 g) and carbon tetrachloride (1.15 ml) were stirred in dimethyl formamide (38 ml) at room temperature for 3 hours. The solution was diluted with methanol (15 ml), then concentrated under reduced pressure. The resulting yellow tar was chromatographed on silica gel, eluting with 4:1 methylene chloride:methanol. The like fractions were combined and concentrated under reduced pressure to afford a purple foam. The presence of triphenylphosphine oxide, as determined by 1H NMR, necessitated a second chromotographic step as above. Yield was 0.43 g of a white foam.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. customThe resulting yellow tar was chromatographed on silica gel
  3. washeluting with 4:1 methylene chloride
  4. concentrationconcentrated under reduced pressure
  5. customto afford a purple foam