HRID1676026

反应详情

EQUATION

反应方程式

HRID 1676026 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of ethyl 3-(1H-benzimidazol-1-yl)-3-(1,1′-biphenyl)-4-yl-2-propenoate (318 mg, 861 μmol) in a mixture of ethanol and water (17:2, 4.2 mL) was added palladium on carbon (47 mg, 10% w/w Pd) and ammonium formate (218 mg, 3.46 mmol). The suspension was brought to reflux for 3 hours, cooled to room temperature, and was filtered through a pad of Celite® and evaporated in vacuo. The residue was purified by flash column chromatography on silica gel, eluting with a mixture of dichloromethane and methanol (97:3) to afford the title compound, [LCMS (Method A, Mobile Phase I) RT=6.51 min, MH+ 371.7].

WORKUP

后处理

  1. temperatureto reflux for 3 hours
  2. filtrationwas filtered through a pad of Celite®
  3. customevaporated in vacuo
  4. customThe residue was purified by flash column chromatography on silica gel
  5. washeluting with a mixture of dichloromethane and methanol (97:3)