HRID66360

反应详情

EQUATION

反应方程式

HRID 66360 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-Chloro-3-nitro-2-pyridone (5.3 g.) was hydrogenated in 225 ml. of ethanol and 6 ml. of acetic acid in the presence of 0.6 g. of 5% palladium-on-carbon. The catalyst was removed by filtration and the filtrate was concentrated to dryness. The residue was dissolved in 75 ml. of pyridine, cooled in ice and treated over 15 minutes with 4.8 g. of benzoyl chloride. The ice bath and reaction mixture were allowed to warm to room temperature spontaneously. The mixture was poured onto 200 g. of ice. On dilution with 500 ml. of water an oil separated which on washing with water solidified (4 g.). The crude 3-benzoylamino-5-chloro-2-pyridone was used directly in the next step.

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated to dryness
  3. dissolutionThe residue was dissolved in 75 ml
  4. temperatureof pyridine, cooled in ice
  5. additiontreated over 15 minutes with 4.8 g
  6. customThe ice bath and reaction mixture
  7. additionThe mixture was poured onto 200 g
  8. customof water an oil separated which
  9. washon washing with water