HRID726708

反应详情

EQUATION

反应方程式

HRID 726708 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl (Z)-[4,4-difluoro-1-[4-(2phenylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-1-benzazepin-5-ylidene]acetate (857 mg) was dissolved in 10 ml of methanol, 2 ml of aqueous solution containing 195 mg of lithium hydroxide monohydrate was added dropwise to the above solution under ice-cooling, and the mixture was stirred at room temperature for 7 hours. After evaporating the solvent under a reduced pressure, 1N hydrochloric acid aqueous solution was added, and the mixture was extracted with chloroform and dried over anhydrous magnesium sulfate. After evaporation of the solvent under a reduced pressure, the resulting residue was recrystallized from ethyl acetatehexane to obtain 633 mg of (Z)-[4,4-difluoro-1-[4-(2-phenylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-1-benzazepin-5-ylidene]acetic acid.

WORKUP

后处理

  1. additionwas added dropwise to the above solution under ice-
  2. temperaturecooling
  3. customAfter evaporating the solvent under a reduced pressure, 1N hydrochloric acid aqueous solution
  4. additionwas added
  5. extractionthe mixture was extracted with chloroform
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customAfter evaporation of the solvent under a reduced pressure
  8. customthe resulting residue was recrystallized from ethyl acetatehexane