HRID1028428

反应详情

EQUATION

反应方程式

HRID 1028428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.67 ml benzylbromide are added dropwise to 1.73 g 3-hydroxy-4-chloro-benzoic acid and 3.04 g potassium carbonate in 10 ml N,N-dimethylformamide, and the reaction mixture is stirred overnight at ambient temperature. Then the reaction mixture is mixed with water and extracted with ethyl acetate. The combined organic phases are dried on magnesium sulphate and evaporated down. The flask residue is taken up in 5 ml of methanol, combined with 3 ml of 10 M aqueous potassium hydroxide solution and stirred for 4 h at 50° C. gerũhrt. The reddish solution is diluted with water and acidified with 3 N aqueous hydrochloric acid. The precipitate formed is suction filtered, washed with water and dried.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. customThe combined organic phases are dried on magnesium sulphate
  3. customevaporated down
  4. stirringstirred for 4 h at 50° C. gerũhrt
  5. additionThe reddish solution is diluted with water
  6. customThe precipitate formed
  7. filtrationfiltered
  8. washwashed with water
  9. customdried