HRID1172682

反应详情

EQUATION

反应方程式

HRID 1172682 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1 g of 4-fluoro-2-methoxy-benzonitrile in 15 mL of dichloroethane was added 1.1 g of aluminum trichloride. The resulting mixture was refluxed for 1 day then poured slowly into water and extracted with ethyl acetate. The organic extracts were washed twice with 10% aqueous solution of sodium hydroxide. The combined basic layers were washed twice with ethyl acetate, acidified with concentrated aqueous solution of hydrochloric acid and extracted three times with ethyl acetate. The combined organic extracts were washed with water, with brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure to give 0.78 g of 4-fluoro-2-hydroxy-benzonitrile as a white solid.

WORKUP

后处理

  1. temperatureThe resulting mixture was refluxed for 1 day
  2. extractionextracted with ethyl acetate
  3. washThe organic extracts were washed twice with 10% aqueous solution of sodium hydroxide
  4. washThe combined basic layers were washed twice with ethyl acetate
  5. extractionextracted three times with ethyl acetate
  6. washThe combined organic extracts were washed with water, with brine
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure