反应详情

温度

120 °C

4,5-Dimethylpyrrole-2-carboxaldehyde (0.27 g, 2.19 mmol) was added to a solution of 2H-1,4-benzothiazin-3(4H)-one (0.36 g, 2.19 mmol) and sodium methoxide (0.118 g, 2.19 mmol) in dry DMF (2 ml). The mixture was heated at 120° C. for 48 h, allowed to cool and poured into ice-water (50 ml). The precipitated solid was collected by filtration, washed with water, then dissolved in ethanol. The insoluble black residue was filtered out and the filtrate was concentrated to dryness under reduced pressure. The product was purified by silica gel chromatography using (98:2) dichloromethane:methanol as the mobile phase.

1. temperatureto cool
2. filtrationThe precipitated solid was collected by filtration
3. washwashed with water
4. dissolutiondissolved in ethanol
5. filtrationThe insoluble black residue was filtered out
6. concentrationthe filtrate was concentrated to dryness under reduced pressure
7. customThe product was purified by silica gel chromatography