HRID465113
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe volatiles were removed at reduced pressure, 10 ml of toluene
- additionwas added
- customthe volatiles again removed
- customThe residue was partitioned between 125 ml of methylene chloride and 25 ml of saturated aqueous sodium carbonate
- customThe organic layer was dried
- customthe solvent removed at reduced pressure
- customgiving an oily solid which
- customwas recrystallized from methylene chloride-hexane