HRID417137
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customThe compound was purified by silica gel chromatography
- washeluting with a gradient of n-heptane:tert-butyl methyl ether (100:0 to 50:50)
- customchromatographed on a preparative HPLC system (Phenomenex Gemini column)