HRID2054014

反应详情

EQUATION

反应方程式

HRID 2054014 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

200 mg (0.49 mmol) of rac.-N-[1-(5-chloro-1H-benzimidazol-2-yl)ethyl]-3-methyl-4-(2,5-dihydropyrrol-1-ylcarbonyl)benzamide and 167 mg (0.73 mmol) of 2,3-dichloro-5,6-dicyano-p-benzoquinone are stirred in 5 mL dioxane for 10 hours at 100° C. Then the solvent is distilled off and the residue is chromatographed on silica gel, eluting with dichloromethane/methanol (0%-6%). Yield: 30 mg (15%); Rf value: 0.62 (silica gel: dichloromethane/ethanol=9:1); C22H19ClN4O2 (406.875); mass spectrum: (M+H)+=407/409 (chlorine isotope).

WORKUP

后处理

  1. distillationThen the solvent is distilled off
  2. customthe residue is chromatographed on silica gel
  3. washeluting with dichloromethane/methanol (0%-6%)