反应详情

A solution of crude [3,8-difluoro-4-hydroxy-7-oxo-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-4-yl]methyl 4-methylbenzenesulfonate (1.2 g, 2.79 mmol) in ethanol (40 mL) was treated with sodium carbonate (889 mg, 8.38 mmol) and 1,1-dimethylethyl 4-piperidinylcarbamate (615 mg, 3.07 mmol). The reaction mixture was stirred at room temperature for 18 hours under argon, evaporated and treated with water (200 mL). The aqueous layer was extracted with a 10% solution of methanol in dichloromethane (3×200 mL) and the combined organic extracts dried over magnesium sulphate and evaporated. The residue was chromatographed eluting with a 0-10% gradient of methanol in dichloromethane affording a yellow solid (1.1 g, 91%).

1. customevaporated
2. additiontreated with water (200 mL)
3. extractionThe aqueous layer was extracted with a 10% solution of methanol in dichloromethane (3×200 mL)
4. dry with materialthe combined organic extracts dried over magnesium sulphate
5. customevaporated
6. customThe residue was chromatographed
7. washeluting with a 0-10% gradient of methanol in dichloromethane affording a yellow solid (1.1 g, 91%)