HRID375528

反应详情

EQUATION

反应方程式

HRID 375528 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-[4-(4-phenylpiperazin-1-yl)but-1-ynyl]benzaldehyde (Example B) (1.28 g), sodium bisulfite (0.4 g) and 1,2-diaminobenzene (0.43 g) is stirred in methanol (50 mL) at reflux for 18 hours. The mixture is filtered and the solvent evaporated. The residue is purified by chromatography on silica gel eluting with 200:8:1 dichloromethane:ethanol:0.880 aqueous ammonia to give 0.70 g of the title compound as a tan solid; mp 247°-248° C.

WORKUP

后处理

  1. temperatureat reflux for 18 hours
  2. filtrationThe mixture is filtered
  3. customthe solvent evaporated
  4. customThe residue is purified by chromatography on silica gel eluting with 200:8:1 dichloromethane