HRID2101316

反应详情

EQUATION

反应方程式

HRID 2101316 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirring solution of 2-chloro-4-(4-chlorophenyl)-3,4′-bipyridine (1.3 g, 4.3 mmol) in pyridine (5 mL) at room temperature under argon was added hydrazine monohydrate (2.5 mL, 51.5 mmol). The reaction mixture was stirred at reflux under argon for 15 h. After cooling the reaction mixture to room temperature, most of the solvent was removed under reduced pressure. Water (25 mL) was added to the residue while stirring and a precipitate formed. The precipitate was collected by filtration and washed with water (15 mL×2). After drying under reduced pressure at elevated temperature, 1.0 g of the title compound was obtained as a yellow solid. HPLC/MS: retention time=1.68 min, [M+H]+=297.

WORKUP

后处理

  1. temperatureat reflux under argon for 15 h
  2. custommost of the solvent was removed under reduced pressure
  3. additionWater (25 mL) was added to the residue
  4. stirringwhile stirring
  5. customa precipitate formed
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with water (15 mL×2)
  8. customAfter drying under reduced pressure at elevated temperature