HRID348599

反应详情

EQUATION

反应方程式

HRID 348599 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The compound (492 mg) obtained in Example 19-1 was dissolved in methanol (5.0 ml) and THF (2.5 ml). Then, the solution was added with activated carbon (49.0 mg) and iron trichloride hexahydrate (manufactured by Kanto Kagaku) (4.90 mg), followed by refluxing under heating for 30 minutes. After the solution was cooled to room temperature, hydrazine monohydrate (0.35 ml) was added to the solution and then the whole was refluxed for 3 hours under heat. After completion of the reaction, the reaction product was filtrated through Celite and the solvent was then distilled off. After the addition of water, chloroform extraction was performed. The extract was dried with anhydrous magnesium sulfate. The solvent was distilled off, thereby obtaining the subject compound (437 mg) as a yellow oily substance.

WORKUP

后处理

  1. temperatureby refluxing
  2. temperatureunder heating for 30 minutes
  3. temperaturethe whole was refluxed for 3 hours
  4. temperatureunder heat
  5. customAfter completion of the reaction
  6. filtrationthe reaction product was filtrated through Celite
  7. distillationthe solvent was then distilled off
  8. additionAfter the addition of water, chloroform extraction
  9. dry with materialThe extract was dried with anhydrous magnesium sulfate
  10. distillationThe solvent was distilled off