HRID2252318

反应详情

EQUATION

反应方程式

HRID 2252318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

A mixture of 2-chloro-benzoic acid N′-(5-bromo-pyridin-2-yl)hydrazide (2.96 g, 9.1 mmol) in POCl3 (15 mL) was heated at 85° C. for 48 hours. The solvent was removed in vacuo, and the residue quenched with saturated Na2CO3 and EtOAc. The layers were separated, and the organic layer concentrated in vacuo to minimal volume. The resulting solid was filtered and purified by flash chromatography to give the title compound (0.85 g, 30%).

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. customthe residue quenched with saturated Na2CO3 and EtOAc
  3. customThe layers were separated
  4. concentrationthe organic layer concentrated in vacuo to minimal volume
  5. filtrationThe resulting solid was filtered
  6. custompurified by flash chromatography