HRID746340

反应详情

EQUATION

反应方程式

HRID 746340 的结构方程式

PROCEDURE

实验过程

Sulfuric acid (230 g) was dropped under stirring for 10 minutes to an ethanol solution (1500 mL) of 3-(4-hydroxyphenyl)propionic acid (1150 g), and refluxed successively for 5 hours. The reaction mixture was concentrated and the obtained concentrated solution was poured into water (1,000 mL) and stirred with addition of ethyl acetate. After separation of the solution, an ethyl acetate layer was neutralized with an aqueous solution of a saturated sodium carbonate, washed with a small amount of water and then dried over anhydrous magnesium sulfate. Ethyl acetate and unreacted ingredients were distilled off from the ethyl acetate layer to obtain concentrates (1,400 g). The concentrates were purified by distillation under a reduced pressure to obtain ethyl 3-(4-hydroxyphenyl)propionate (1,144 g). The boiling point was 160° C./4.0 hPa.

WORKUP

后处理

  1. temperaturerefluxed successively for 5 hours
  2. concentrationThe reaction mixture was concentrated
  3. additionthe obtained concentrated solution was poured into water (1,000 mL)
  4. customAfter separation of the solution
  5. washwashed with a small amount of water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationEthyl acetate and unreacted ingredients were distilled off from the ethyl acetate layer
  8. customto obtain concentrates (1,400 g)
  9. distillationThe concentrates were purified by distillation under a reduced pressure