HRID1416549

反应详情

EQUATION

反应方程式

HRID 1416549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the solution of 1,1-dimethylhydrazine (0.6 mL) in methanol (15 mL) was added, in portions, a suspension of N-(4-chloro-3-formylphenyl)-2-methyl-3-furancarboxamide (2 g) in methanol (30 mL) at such a rate that the temperature of the solution was maintained at -5° C. to 0° C. The resultant mixture was stirred overnight at ambient temperature. Acetic acid (0.1 mL) was then added to the reaction mixture which was then refluxed for 30 minutes, solvent was evaporated and the reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with water, dried (MgSO4) filtered and evaporated to produce N-[4-chloro-3-[dimethylhydrazono)methyl]phenyl]-2-methyl 3-furancarboxamide as a white solid, m.p. 109-111° C.

WORKUP

后处理

  1. temperaturewas maintained at -5° C. to 0° C
  2. temperaturewas then refluxed for 30 minutes
  3. customsolvent was evaporated
  4. additionthe reaction mixture was poured into water
  5. extractionextracted with ethyl acetate
  6. washThe organic layer was washed with water
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. customevaporated