HRID131587

反应详情

EQUATION

反应方程式

HRID 131587 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A suspension of 3,4-dihydroxybenzaldehyde (5.0 gm, 0.0362 mol), anhydrous potassium carbonate (6.0 gm, 0.0434 mol) and cyclopentyl bromide (6.5 gm, 0.0434 mol) in dry DMF (50 ml) was heated and stirred at 80° C. for 24 hrs. Reaction mixture was then cooled and diluted with water (500 ml), acidified with 1N HCl and extracted with ethyl acetate (3×100 ml). The ethyl acetate extract was washed 5% sodium bicarbonate and brine and dried over anhydrous sodium sulfate. The dried extract on concentration afforded a residue which was purified by silica gel chromatography using 10% ethyl acetate in petroleum ether as the eluent to provide 5.0 gm of the title product as white solid. mp: 87-89° C.

WORKUP

后处理

  1. temperaturewas heated
  2. customReaction mixture
  3. temperaturewas then cooled
  4. extractionextracted with ethyl acetate (3×100 ml)
  5. extractionThe ethyl acetate extract
  6. washwas washed 5% sodium bicarbonate and brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. extractionThe dried extract on concentration
  9. customafforded a residue which
  10. customwas purified by silica gel chromatography