反应详情

温度

0 °C

To a solution of 5-bromopyridin-3-amine (1.73 g, 10 mmol) and triethylamine (4.05 g, 40 mmol) in DCM (100 mL) was added a solution of ethanesulfonyl chloride (3.86 g, 30 mmol) in DCM (20 mL) at 0° C. The mixture was stirred at 0° C. for 1 h. 1N NaOH in water (10 mL) and methanol (20 mL) were added and the mixture was concentrated in vacuo, Silica gel (20 g) and DCM (100 mL) were added and the mixture was concentrated in vacuo. The residue was purified by silica chromatography eluting with a 0 to 5% MeOH-DCM gradient to give N-(5-bromopyridin-3-yl)ethanesulfonamide. ESI-MS: m/z 265.2, 267.2 (M+H)+.

1. concentrationthe mixture was concentrated in vacuo, Silica gel (20 g) and DCM (100 mL)
2. additionwere added
3. concentrationthe mixture was concentrated in vacuo
4. customThe residue was purified by silica chromatography
5. washeluting with a 0 to 5% MeOH-DCM gradient