反应详情

The title compound was prepared in analogy to Example 4, intermediate, from 2-[2-(4-chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclopentyl-ethanol, 3,5-dimethyl-4-hydroxybenzonitrile (commercially available), tri-n-butylposphine and N′N′N′N-tetramethylazodicarboxamide. The compound was purified by silica gel chromatography using a MPLC system (CombiFlash Companion, Isco Inc.) eluting with a gradient of n-heptane:ethyl acetate (100:0 to 60:40). The product containing fractions were pooled and evaporated. The resulting light yellow foam was dissolved in acetonitrile, upon which crystallisation occurred. The suspension was filtered, washed with a small amount of acetonitrile and dried under high vacuum. White solid (34%). MS (Turbo Spray): m/z=506.182 [M+H].

1. customThe compound was purified by silica gel chromatography
2. washeluting with a gradient of n-heptane:ethyl acetate (100:0 to 60:40)
3. additionThe product containing fractions
4. customevaporated
5. dissolutionThe resulting light yellow foam was dissolved in acetonitrile, upon which crystallisation
6. filtrationThe suspension was filtered
7. washwashed with a small amount of acetonitrile
8. customdried under high vacuum