反应详情

A mixture of 2-{4-[6-chloro-2-(1-chloro-1-methylethyl)-5-(trifluoromethyl)-1H-benzimidazol-1-yl]phenyl}ethyl acetate (step 1, 273 mg, 0.68 mmol), sodium azide (88 mg, 1.36 mmol), KI (112 mg, 0.68 mmol) in DMF (8 ml) was stirred under nitrogen at room temperature for 5.5 h. The reaction mixture was poured into water (5 ml) and the aqueous mixture was extracted with ethyl acetate(30 ml). The organic layer was washed with water (5 ml) and brine (10 ml), then dried (Na2SO4). After removal of solvent, the crude product was purified by flash column chromatography eluting with hexane/ethyl acetate (2/1) to afford 133 mg (42%) of the title compound as yellow oil.

1. extractionthe aqueous mixture was extracted with ethyl acetate(30 ml)
2. washThe organic layer was washed with water (5 ml) and brine (10 ml)
3. dry with materialdried (Na2SO4)
4. customAfter removal of solvent
5. customthe crude product was purified by flash column chromatography
6. washeluting with hexane/ethyl acetate (2/1)