HRID417137

反应详情

EQUATION

反应方程式

HRID 417137 的结构方程式

PROCEDURE

实验过程

The title compound was prepared in analogy to Example 4, intermediate, from 2-[2-(4-chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclohexyl-ethanol (Example 1, intermediate c), 3,5-difluorobenzonitrile (commercially available), triphenylphosphine and di-tert-butyl azodicarboxylate. The compound was purified by silica gel chromatography using a MPLC system (CombiFlash Companion, Isco Inc.) eluting with a gradient of n-heptane:tert-butyl methyl ether (100:0 to 50:50). The product-containing fractions were pooled and chromatographed on a preparative HPLC system (Phenomenex Gemini column) using a gradient of acetonitrile and water. Colorless foam (49%). MS (Turbo Spray): m/z=528.1 [M+H].

WORKUP

后处理

  1. customThe compound was purified by silica gel chromatography
  2. washeluting with a gradient of n-heptane:tert-butyl methyl ether (100:0 to 50:50)
  3. customchromatographed on a preparative HPLC system (Phenomenex Gemini column)