HRID1982749

反应详情

EQUATION

反应方程式

HRID 1982749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A solution comprising 14 g of allyl (4-chlorobutyl) ether, 14 g of 4-hydroxybenzoic acid, 14 g of potassium carbonate and 50 ml of dimethylformamide was stirred at 90° C. for 3 hours. Water was added to it, and extracted with toluene, and the toluene layer was well washed with water, and toluene was evaporated away. 20 g of sodium hydroxide, 50 ml of water and 200 ml of ethanol were added to the resulting residue, and refluxed for 2 hours. Ethanol was evaporated away, and hydrochloric acid was added to make it acidic, and then extracted with diethyl ether and dried with anhydrous magnesium sulfate. The solvent was evaporated away, and the resulting residue was recrystallized from a mixed solvent of ethanol and water to obtain 29 g of 4-(4-allyloxybutyloxy)benzoic acid.

WORKUP

后处理

  1. extractionextracted with toluene
  2. washthe toluene layer was well washed with water, and toluene
  3. customwas evaporated away
  4. addition20 g of sodium hydroxide, 50 ml of water and 200 ml of ethanol were added to the resulting residue
  5. temperaturerefluxed for 2 hours
  6. customEthanol was evaporated away
  7. additionhydrochloric acid was added
  8. extractionextracted with diethyl ether
  9. dry with materialdried with anhydrous magnesium sulfate
  10. customThe solvent was evaporated away
  11. customthe resulting residue was recrystallized from a mixed solvent of ethanol and water