HRID1844946

反应详情

EQUATION

反应方程式

HRID 1844946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the above 0.5 g (2.4 mmol) N-(4-phenyl-1H-imidazol-2-yl)-acetamide in MeOH (20 mL) was added water (20 mL) and conc. H2SO4 (1 mL). The mixture was refluxed under nitrogen for 2 days. After cooling to rt, the organic solvent was removed under vacuum. The reaction mixture was neutralized with saturated sodium bicarbonate aq. solution (50 mL) and extracted with ethyl acetate (150 mL). The organic layer was dried and condensed. The residue was purified by a flash column chromatography eluting with EtOAc then EtOAc/MeOH=7:1 to give 4-phenyl-1H-imidazol-2-ylamine (160 mg, 41%). LCMS: 160 (M+1)+.

WORKUP

后处理

  1. temperatureThe mixture was refluxed under nitrogen for 2 days
  2. customthe organic solvent was removed under vacuum
  3. extractionextracted with ethyl acetate (150 mL)
  4. customThe organic layer was dried
  5. customcondensed
  6. customThe residue was purified by a flash column chromatography
  7. washeluting with EtOAc