反应详情

温度

68 °C

A 1 mL vial was charged with N-(2,5-Dimethyl-2H-pyrazol-3-yl)-2-{3-[1-hydroxy-meth-(Z)-ylidene]-2-oxo-2,3-dihydro-1H-indol-6-ylsulfanyl}-benzamide (as prepared below; 55 mg, 0.135 mmol), 4-(4-methyl-piperazin-1-yl)-phenylamine (25.8 mg, 0.138 mmol), and THF (1 mL). This reaction mixture was stirred for 24 h at 68° C. Subsequently, the reaction mixture was cooled to room temperature and concentrated in vacuo. The crude residue was re-suspended in EtOAc (5 mL) and extracted with H2O (˜5 mL). The organic layer was concentrated in vacuo and the residue was chromatographed via flash silica gel chromatography (gradient of 1-10% MeOH in CHCl3) afforded the title compound in 35% yield (27 mg, 0.047 mmol).

1. temperatureSubsequently, the reaction mixture was cooled to room temperature
2. concentrationconcentrated in vacuo
3. extractionextracted with H2O (˜5 mL)
4. concentrationThe organic layer was concentrated in vacuo
5. customthe residue was chromatographed via flash silica gel chromatography (gradient of 1-10% MeOH in CHCl3)