反应详情

To a solution of benzo[b]thiophene-2-sulfonic acid [2-(5-ethenesulfonyl-2-methoxybenzenesulfonylamino)phenyl] amide (0.2 mmol, prepared as in Example 19) in dry THF (2 mL) was added 0.2 mL of 1-methylpiperazine. The resulting reaction mixture was stirred at room temperature for 1 h. The reaction mixture was diluted with DCM (10 mL) and washed with saturated sodium chloride aqueous solution (25 mL). The organic phase was dried over anhydrous sodium sulfate and concentrated under vacuum. The residue obtained was purified by flash column chromatography eluting with EtOAc then DCM/methanol/AcOH (100:2:1 to 100:10:2) to furnish 118 mg of benzo[b]thiophene-2-sulfonic acid {2-[2-methoxy-5-(2-pyrrolidin-1-yl-ethanesulfonyl)-benzenesulfonylamino]-phenyl}-amide. LC: Tr 0.84 min; MS: 666.0 (M+1)+.

1. customThe resulting reaction mixture
2. washwashed with saturated sodium chloride aqueous solution (25 mL)
3. dry with materialThe organic phase was dried over anhydrous sodium sulfate
4. concentrationconcentrated under vacuum
5. customThe residue obtained
6. customwas purified by flash column chromatography
7. washeluting with EtOAc