反应详情

To a solution of 2-{4-[2-(1-amino-1-methylethyl)-6-chloro-5-(trifluoromethyl)-1H-benzimidazol-1-yl]phenyl}ethyl acetate (step 3, 121 mg, 0.27 mmol) in dichloromethane (5 ml) was added acetyl chloride (0.02 ml, 0.3 mmol). The reaction mixture was stirred at room temperature for 7 h. To the reaction mixture was added water (5 ml) and the aqueous mixture was extracted with dichloromethane (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 CH2Cl2/methanol (10/1) to afford 76 mg (57%) of the title compound as white amorphous.

1. extractionthe aqueous mixture was extracted with dichloromethane (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 CH2Cl2/methanol (10/1)