HRID1266937

反应详情

EQUATION

反应方程式

HRID 1266937 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Next, a flask was loaded with 3-(N,N-diethylamino)phenol (1.7 g), dimethylformamide (14 ml), acetic acid (5 ml) and iodine (0.24 g), and they were mixed, followed by addition of 3,5-dichloro-2-hydrazinopyridine (1.6 g) to the flask with stirring. Then, to this, a 30% hydrogen peroxide water (2.4 g) was dropwise added in 90 minutes and the mixture was stirred overnight. The reaction mixture was filtrated, and ether and water were added to the filtrate, followed by stirring. After stirring, the ether layer was collected and condensed to precipitate crystals. The crystals were filtrated for collection and dried to give intended crystals (0.54 g).

WORKUP

后处理

  1. additionwere mixed
  2. stirringthe mixture was stirred overnight
  3. filtrationThe reaction mixture was filtrated
  4. additionether and water were added to the filtrate
  5. stirringby stirring
  6. stirringAfter stirring
  7. customthe ether layer was collected
  8. customcondensed
  9. customto precipitate crystals
  10. filtrationThe crystals were filtrated for collection
  11. customdried
  12. customto give