反应详情

1,1′-thiocarbonyldiimidazole (1.13 g, 6.25 mmol) is added by portions to a solution of 4-(trifluoromethoxy)-ortho-phenylenediamine (1 g, 5.2 mmol) in 5 ml of tetrahydrofuran and the mixture is stirred at room temperature for 16 hours. The reaction mixture is then concentrated under reduced pressure and the residue is dissolved in 100 ml of ethyl acetate and washed with water (2×30 ml). The organic phase is then dried over MgSO4, filtered and concentrated. The residue is triturated in diisopropylether and pentane and dried under vacuum to yield 1.26 g of 2-mercapto-5-trifluoromethoxy-benzimidazole as a yellow powder. Quantitative yield. Analytical LC/MS (method B): retention time=3.69 min. m/z=235.67 (positive ion mode).

1. concentrationThe reaction mixture is then concentrated under reduced pressure
2. dissolutionthe residue is dissolved in 100 ml of ethyl acetate
3. washwashed with water (2×30 ml)
4. dry with materialThe organic phase is then dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue is triturated in diisopropylether
8. dry with materialpentane and dried under vacuum