HRID1248361

反应详情

EQUATION

反应方程式

HRID 1248361 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.0 g of 4-benzoyl-5-hydroxybenzocyclobutene-1-methanol is dissolved in 50 ml of acetic acid and then 4.0 g of chromium trioxide are added in portions. The whole is stirred for 16 hours at 40°, concentrated to dryness by evaporation under reduced pressure, taken up in 20 ml of water and extracted by shaking with 80 ml of dichloromethane. The organic phase is dried over magnesium sulphate and concentrated by evaporation. After recrystallisation of the residue from ether/hexane, 4-benzoyl-5-hydroxybenzocyclobutene-1-carboxylic acid is obtained having a melting point of 167°-169°.

WORKUP

后处理

  1. concentrationconcentrated to dryness by evaporation under reduced pressure
  2. extractionextracted
  3. stirringby shaking with 80 ml of dichloromethane
  4. dry with materialThe organic phase is dried over magnesium sulphate
  5. concentrationconcentrated by evaporation
  6. customAfter recrystallisation of the residue from ether/hexane