HRID1418097
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customequipped with a Dean and Stark
- temperatureThe reactants were then cooled
- customevaporated into silica
- customThe silica was formed into a column which
- washwas then developed by elution with hexane containing
- temperatureincreasing amounts of dichloromethane
- customThe product was obtained from fractions