HRID465113

反应详情

EQUATION

反应方程式

HRID 465113 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A 440 mg portion of 2-chloro-3,3'-bipyridine and 0.73 ml of anhydrous hydrazine were dissolved in 15 ml of pyridine and heated at 110° C. for 3 days. The volatiles were removed at reduced pressure, 10 ml of toluene was added and the volatiles again removed. The residue was partitioned between 125 ml of methylene chloride and 25 ml of saturated aqueous sodium carbonate. The organic layer was dried and the solvent removed at reduced pressure, giving an oily solid which was recrystallized from methylene chloride-hexane, giving 2-hydrazino-3,3'-bipyridine as a tan powder, mp 104.5°-107° C.

WORKUP

后处理

  1. customThe volatiles were removed at reduced pressure, 10 ml of toluene
  2. additionwas added
  3. customthe volatiles again removed
  4. customThe residue was partitioned between 125 ml of methylene chloride and 25 ml of saturated aqueous sodium carbonate
  5. customThe organic layer was dried
  6. customthe solvent removed at reduced pressure
  7. customgiving an oily solid which
  8. customwas recrystallized from methylene chloride-hexane