HRID467800

反应详情

EQUATION

反应方程式

HRID 467800 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15.01 g (89.9 mmol) 4-nitrobenzoic acid are suspended in 500 mL MeCN and then combined with 15.03 g (108.7 mmol, 1.2 eq) potassium carbonate. 15.4 g (90.4 mmol, 1.01 eq) benzylbromide are added dropwise with stirring and the reaction mixture is heated for 5 h with stirring at 60° C. It is combined with 750 mL distilled water, extracted 4 times with 250 mL of EE and after the organic phases have been combined dried on sodium sulphate. After all the volatile constituents have been eliminated in vacuo the crude product is suspended twice in succession in toluene and evaporated down in vacuo. 20.6 g (80.1 mmol) benzyl 4-nitrobenzoate are obtained, which is used in the next step without any further purification.

WORKUP

后处理

  1. temperaturethe reaction mixture is heated for 5 h
  2. stirringwith stirring at 60° C
  3. distillationdistilled water
  4. extractionextracted 4 times with 250 mL of EE
  5. customafter the organic phases have been combined dried on sodium sulphate
  6. customevaporated down in vacuo