反应详情

5-Amino-2-(1-benzothien-2-yl)benzamide (Example 8A, 886 mg) and triethylamine (650 mg) are introduced into DCM (20 ml) at 0° C., and 2-bromobutyryl bromide (1000 mg) is slowly added. The reaction mixture is warmed to RT and then stirred overnight. The reaction mixture is subsequently diluted with DCM (100 ml) and washed with 5% strength potassium bisulfate solution (twice 50 ml), dried (sodium sulfate) and concentrated in a rotary evaporator. The residue is chromatographed on silica gel (eluent cyclohexane-ethyl acetate 10:1 to 1:1). After concentration of the relevant fraction, 607 mg (47% of theory) of product are isolated.

1. washwashed with 5% strength potassium bisulfate solution (twice 50 ml)
2. dry with materialdried (sodium sulfate)
3. concentrationconcentrated in a rotary evaporator
4. customThe residue is chromatographed on silica gel (eluent cyclohexane-ethyl acetate 10:1 to 1:1)
5. customAfter concentration of the relevant fraction, 607 mg (47% of theory) of product are isolated