HRID355597

反应详情

EQUATION

反应方程式

HRID 355597 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

4-Chlorobutyl acetate (276.6 g; 1.8 mol) is added to a solution of ethyl 4-hydroxybenzoate (249 g; 1.5 mol), potassium iodide (3 g) and potassium carbonate (248 g; 1.8 mol) in dimethylformamide (2 l), and the mixture is stirred at 90° C. for 11 hours. The reaction mixture is transferred into 5 l of ice water, and the resultant precipitate is filtered off with suction and washed with 4 to 5 l of ice water. The crude product is dissolved in 3 l of ethanol, potassium hydroxide (400 g) is added, and the mixture is refluxed for 3 hours. The reaction mixture is transferred into 6 l of ice water, and acidified by means of concentrated hydrochloric acid, and the precipitate is filtered off, washed with water until neutral and then dried.

WORKUP

后处理

  1. filtrationthe resultant precipitate is filtered off with suction
  2. washwashed with 4 to 5 l of ice water
  3. dissolutionThe crude product is dissolved in 3 l of ethanol
  4. additionpotassium hydroxide (400 g) is added
  5. temperaturethe mixture is refluxed for 3 hours
  6. filtrationthe precipitate is filtered off
  7. washwashed with water until neutral and
  8. customthen dried