HRID53483

反应详情

EQUATION

反应方程式

HRID 53483 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 2,4,6-triiodophenol (0.78 g, 1.65 mmol) and potassium carbonate (0.25 g, 1.82 mmol, 1.1 eq) in 5 ml of dimethylformamide was heated at 60° C. for 1 hr, cooled and then 3,3-diphenylpropyl bromide (0.5 g, 1.82 mmol) was added. After stirring for 30 minutes at room temperature the mixture was heated at 60° C. for 24 hrs. The mixture was then cooled, poured into water and the crude product was isolated by ethyl acetate extraction. The product was purified by silica gel chromatography (2.5% ethyl acetate-hexanes) followed by recrystallization from hexanes to give 0.53 g (48%) of a solid. Mp: 120°-121° C.

WORKUP

后处理

  1. temperaturecooled
  2. temperaturewas heated at 60° C. for 24 hrs
  3. temperatureThe mixture was then cooled
  4. customThe product was purified by silica gel chromatography (2.5% ethyl acetate-hexanes)
  5. customfollowed by recrystallization from hexanes