HRID348683

反应详情

EQUATION

反应方程式

HRID 348683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound (1.24 g) obtained in Example 87-1 was dissolved in methanol (12 ml) and THF (6.2 ml) and added with activated carbon (124 mg) and iron trichloride hexahydrate (12.4 mg), followed by thermal reflux for 0.5 hour. After standing to cool, the solution was added with hydrazine monohydrate (0.89 ml) and then subjected to thermal reflux for 3 hours. After completion of the reaction, the resultant was filtrated through Celite and the solvent was then distilled off. The residue was dissolved in chloroform and washed with water. The solution was dried with anhydrous magnesium sulfate. The solvent was distilled off, thereby obtaining the subject compound (1.15 g) as a yellow viscous liquid.

WORKUP

后处理

  1. temperatureby thermal reflux for 0.5 hour
  2. temperatureto cool
  3. temperaturethermal reflux for 3 hours
  4. customAfter completion of the reaction
  5. filtrationthe resultant was filtrated through Celite
  6. distillationthe solvent was then distilled off
  7. dissolutionThe residue was dissolved in chloroform
  8. washwashed with water
  9. dry with materialThe solution was dried with anhydrous magnesium sulfate
  10. distillationThe solvent was distilled off