HRID1266935

反应详情

EQUATION

反应方程式

HRID 1266935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Next, a reaction flask was loaded with 3-(N,N-diethlyamino)phenol (1.3 g), dimethylformamide (9 ml), acetic acid (3 ml) and iodine (0.14 g), and they were mixed, followed by addition of 3-chloro-2-hydrazino-5-trifluoromethylpyridine (1.0 g) to the flask with stirring. Then, to this mixture, a 30 % hydrogen peroxide water (1.4 g) was dropwise added in one hour and the mixture was stirred overnight. Water was added to this reaction mixture, followed by extraction with ether. The organic layer was condensed to precipitate crystals. The crystals were filtrated for collection and dried to give intended crystals (0.5 g).

WORKUP

后处理

  1. additionwere mixed
  2. stirringthe mixture was stirred overnight
  3. extractionfollowed by extraction with ether
  4. customcondensed
  5. customto precipitate crystals
  6. filtrationThe crystals were filtrated for collection
  7. customdried
  8. customto give