HRID465120

反应详情

EQUATION

反应方程式

HRID 465120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5.0 g of 2'-chloro-2,4'-bipyridine, 5 ml of anhydrous hydrazine and 100 ml of pyridine was refluxed. Additional 5 ml portions of anhydrous hydrazine were added after 18, 36 and 54 hours of refluxing. The solution was then refluxed for an additional 48 hours and the solvent removed under vacuum. The solid was dissolved in methylene chloride, treated with activated carbon, filtered and the filtrate concentrated to dryness. The residue was triturated with hexane, giving crystals which were recrystallized from methylene chloride-hexane, giving 2'-hydrazino-2,4'-bipyridine as yellow crystals, mp 120°-121° C.

WORKUP

后处理

  1. temperaturewas refluxed
  2. temperatureof refluxing
  3. temperatureThe solution was then refluxed for an additional 48 hours
  4. customthe solvent removed under vacuum
  5. dissolutionThe solid was dissolved in methylene chloride
  6. additiontreated with activated carbon
  7. filtrationfiltered
  8. concentrationthe filtrate concentrated to dryness
  9. customThe residue was triturated with hexane
  10. customgiving crystals which
  11. customwere recrystallized from methylene chloride-hexane