反应详情

To a stirred solution of N-[4-(3-chloro-phenyl)-5-(1-cyclopentyl-3-methyl-2-oxo-2,3-dihydro-1H-benzoimidazol-5-yl)-1H-imidazol-2-yl]-acetamide (prepared as described above, 102 mg) in methanol:water (1:1, 10 mL) was added concentrated sulfuric acid (ca. 0.5 mL). The mixture was heated to reflux for 4 hours, after which the reaction was cooled to room temperature and the concentrated in vacuo. The resulting aqueous solution was diluted with water and the pH was adjusted to 10 with aqueous ammonium hydroxide. The mixture was filtered and the resulting white powder was taken up in 1M HCl in ether and concentrated in vacuo to afford 70 mg of the title compound as the HCl salt. MS (M+1)=408.1 (free base).

1. temperatureThe mixture was heated
2. temperatureto reflux for 4 hours
3. concentrationthe concentrated in vacuo
4. additionThe resulting aqueous solution was diluted with water
5. filtrationThe mixture was filtered
6. concentrationconcentrated in vacuo