反应详情

2-(1-Benzothien-2-yl)-5-[(2-bromobutanoyl)amino]benzamide (Example 9A; 50 mg) is introduced into DMF (1 ml) and, after addition of 3-mercapto-1,2,4-triazine (15 mg) and cesium carbonate (78 mg), stirred at RT overnight. The reaction mixture is mixed with ethyl acetate (50 ml) and 0.5N hydrochloric acid (50 ml), the aqueous phase is extracted with ethyl acetate (twice 50 ml), and the combined organic phases are washed with saturated sodium chloride solution (twice 100 ml). The organic phase is dried over magnesium sulfate and concentrated in a rotary evaporator. The residue is purified on a preparative HPLC. 14 mg (26% of theory) of the title compound are obtained.

1. extractionthe aqueous phase is extracted with ethyl acetate (twice 50 ml)
2. washthe combined organic phases are washed with saturated sodium chloride solution (twice 100 ml)
3. dry with materialThe organic phase is dried over magnesium sulfate
4. concentrationconcentrated in a rotary evaporator
5. customThe residue is purified on a preparative HPLC