反应详情

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0 °C

A solution of N-[({2-[4-(5-acetyl-2-ethyl-1H-benzimidazol-1-yl)phenyl]ethyl}amino)carbonyl]-4-methylbenzenesulfonamide (Example 78, 100 mg, 0.19 mmol) in tetrahydrofurane (15 ml) was added MeMgI (1.2 ml, 0.99 mmol) dropwise under nitrogen at 0° C. The mixture was stirred at 0° C. for 1 h and then was stirred at rt for 30 min. The mixture was added water (10 ml) and extracted with CH2Cl2(50 ml). The organic layer was washed with brine (10 ml), then dried (Na2SO4). After removal of solvent, the crude product was purified by flash column chromatography eluting with CH2Cl2:methanol (30:1/20:1/10:1) to afford 100 mg (97%) of the title compound as white solids.

1. stirringwas stirred at rt for 30 min
2. extractionextracted with CH2Cl2(50 ml)
3. washThe organic layer was washed with brine (10 ml)
4. dry with materialdried (Na2SO4)
5. customAfter removal of solvent
6. customthe crude product was purified by flash column chromatography
7. washeluting with CH2Cl2:methanol (30:1/20:1/10:1)