反应详情

温度

60 °C

The purified intermediate 2-(3-fluoro-4-methylsulfonyl-benzyl)-isoindole-1,3-dione (5.50 g, 15.6 mmol) is dissolved in a mixture of methanol (250 mL) and dichloromethane (250 mL). Hydrazine hydrate (4.6 g, 78.4 mmol) is added, and the mixture is stirred at 60° C. for 3 h. The mixture is filtered, and the filtrate is treated with water. The mixture is extracted with ethyl acetate, and the organic layer is dried over Na2SO4 and concentrated under reduced pressure. The residue is purified by preparative reversed-phase HPLC (Luna C18 250*50 mm, gradient of acetonitrile in water, 0.1% TFA). Yield: 3.1 g (81% of theory); ESI mass spectrum: [M+H]+=204; Retention time HPLC: 0.17 min (X012_S01).

1. filtrationThe mixture is filtered
2. additionthe filtrate is treated with water
3. extractionThe mixture is extracted with ethyl acetate
4. dry with materialthe organic layer is dried over Na2SO4
5. concentrationconcentrated under reduced pressure
6. customThe residue is purified by preparative reversed-phase HPLC (Luna C18 250*50 mm, gradient of acetonitrile in water, 0.1% TFA)
7. custom0.17 min (X012_S01)