HRID37493

反应详情

EQUATION

反应方程式

HRID 37493 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 5 ml of ethanol was dissolved 160 mg of 3,4-diethoxycarbonyl-2-fluoro-5-nitro-6-phenylpyridine, and 120 mg (5 eq.) of reduced iron was added to the solution, followed by addition of 0.5 ml (20 eq.) of acetic acid. After the mixture was refluxed for 30 minutes, the solvent was distilled off. The residue was neutralized with sodium hydrogencarbonate, followed by extraction with ethyl acetate. After the precipitate was removed by filtration, the obtained organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried. Then, the solvent was distilled off.

WORKUP

后处理

  1. additionwas added to the solution
  2. temperatureAfter the mixture was refluxed for 30 minutes
  3. distillationthe solvent was distilled off
  4. extractionfollowed by extraction with ethyl acetate
  5. customAfter the precipitate was removed by filtration
  6. washthe obtained organic layer was washed with water
  7. dry with materiala saturated aqueous solution of sodium chloride, and dried
  8. distillationThen, the solvent was distilled off