HRID2213070

反应详情

EQUATION

反应方程式

HRID 2213070 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Hydrazine hydrate (0.3 mL, 5.9 mmol) was added to a stirred solution of 5-chloro-2-phenyl-isonicotinonitrile (420 mg, 1.9 mmol) in pyridine (5 mL). The reaction mixture was stirred at reflux for 3 hours, cooled and the resulting solid was filtered and dried in vacuo, affording a crude residue. Purification by column chromatography using a gradient elution of 0–5% methanol in dichloromethane as eluent afforded the title compound as a solid.

WORKUP

后处理

  1. temperatureat reflux for 3 hours
  2. temperaturecooled
  3. filtrationthe resulting solid was filtered
  4. customdried in vacuo
  5. customaffording a crude residue
  6. customPurification by column chromatography
  7. washa gradient elution of 0–5% methanol in dichloromethane as eluent