反应详情

温度

10 °C

To a stirred solution at room temperature of chalcone XXIIIa (1.29 g, 5.13 mmol) in DMF (20 ml) was added phenylsulfonylhydrazine (1.76 g, 10.26 mmol). The reaction mixture was stirred at 10° C. for 15 h, cooled and concentrated. The remained oily residue was partitioned between a saturated aqueous solution of NH4Cl and AcOEt. After separation, the organic layer was dried, partially evaporated and filtered. The filtrate was purified by flash chromatography on silica gel (AcOEt/hexane:50/50□75/25) to form a material which after a second column purification (MeOH/CH2Cl2:5/95) afford the title compound XXVIa (400 mg, 1.59 mmol, 31% yield).

1. temperaturecooled
2. concentrationconcentrated
3. customThe remained oily residue was partitioned between a saturated aqueous solution of NH4Cl and AcOEt
4. customAfter separation
5. customthe organic layer was dried
6. custompartially evaporated
7. filtrationfiltered
8. customThe filtrate was purified by flash chromatography on silica gel (AcOEt/hexane:50/50□75/25)
9. customto form a material which
10. customafter a second column purification (MeOH/CH2Cl2:5/95)