反应详情

温度

-78 °C

tert-Butyl 2-{4-[(ethylsulfonyl)amino]phenyl}-1H-pyrrole-1-carboxylate (3.0 g, 8.58 mmol) was dissolved in tetrahydrofuran (85 mL) and cooled to −78° C., followed by the slow addition of chlorosulfonyl isocyanate. After tert-Butyl 2-{4-[(ethylsulfonyl)amino]phenyl}-1H-pyrrole-1-carboxylate was consumed, dimethyl formamide (6.86 mL) was added and the solution allowed to warm to room temperature. After 2 hours, the mixture was cooled and partitioned between water and diethyl ether. The combined organic layers were dried over magnesium sulfate, and concentrated. The residue was purified by silica gel flash chromatography (hexane/ethyl acetate; 7:3) to afford the title compound (1.84 g, 57%). The title compound was used immediately in the next step.

1. customAfter tert-Butyl 2-{4-[(ethylsulfonyl)amino]phenyl}-1H-pyrrole-1-carboxylate was consumed
2. additiondimethyl formamide (6.86 mL) was added
3. temperatureto warm to room temperature
4. temperaturethe mixture was cooled
5. custompartitioned between water and diethyl ether
6. dry with materialThe combined organic layers were dried over magnesium sulfate
7. concentrationconcentrated
8. customThe residue was purified by silica gel flash chromatography (hexane/ethyl acetate; 7:3)