反应详情

NaH (7 mg, 0.3 mmol) is added to a solution of 23 μl (0.30 mmol) 4-methylpyrazole in 2 ml DMF. The resulting mixture is stirred at room temperature for 1 h, then 119 mg (0.23 mmol) methanesulfonic acid 4-bromo-2-(4-isopropyl-phenyl)-7-methoxy-1-(2-methoxy-ethyl)-1H-benzoimidazol-5-ylmethyl ester is added. Stirring is continued for 20 h. After that the reaction mixture is poured on water and extracted (3×) with ethyl acetate. The combined organic layers are washed with water (2×) and brine, dried over MgSO4, filtered and concentrated in vacuo. The residue is purified by flash-chromatography on silica gel (dichloromethane:isopropanol=95:5) to afford 80 mg of the title compound as a white foam.

1. stirringStirring
2. waitis continued for 20 h
3. additionAfter that the reaction mixture is poured on water
4. extractionextracted (3×) with ethyl acetate
5. washThe combined organic layers are washed with water (2×) and brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe residue is purified by flash-chromatography on silica gel (dichloromethane:isopropanol=95:5)