HRID2186871

反应详情

EQUATION

反应方程式

HRID 2186871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

45 gm of succinic anhydride and 130.7 gm of aluminum chloride were added to 57 gm of difluorobenzene, and the mixture was heated under reflux for 4 hours. Upon the addition of 200 ml of 1% hydrochloric acid aqueous solution, the reaction mixture was extracted with chloroform, washed. with water, and dried over anhydrous sodium sulfate. The solvent was evaporated and the residue was subjected to silica gel column chromatography using a chloroform-methanol (30:1) mixed solvent as an eluant to obtain fractions containing the target compound. The fractions were concentrated to produce 30 gm of the title compound.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 4 hours
  3. extractionthe reaction mixture was extracted with chloroform
  4. washwashed
  5. dry with materialwith water, and dried over anhydrous sodium sulfate
  6. customThe solvent was evaporated
  7. additionmixed solvent as an eluant
  8. customto obtain fractions
  9. additioncontaining the target compound
  10. concentrationThe fractions were concentrated