HRID1418097

反应详情

EQUATION

反应方程式

HRID 1418097 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-bromo-2-formylthiophene (3.89 parts, 0.02M) was heated at reflux with dry ethyleneglycol (1.6 parts) toluene (25 parts) and p-toluene sulphonic acid (0.1 parts) in a vessel equipped with a Dean and Stark separator for 16 hours. The reactants were then cooled and evaporated into silica. The silica was formed into a column which was then developed by elution with hexane containing increasing amounts of dichloromethane. The product was obtained from fractions containing 10-60% dichloromethane as a pale straw-coloured oil (4.42 parts).

WORKUP

后处理

  1. customequipped with a Dean and Stark
  2. temperatureThe reactants were then cooled
  3. customevaporated into silica
  4. customThe silica was formed into a column which
  5. washwas then developed by elution with hexane containing
  6. temperatureincreasing amounts of dichloromethane
  7. customThe product was obtained from fractions