反应详情

温度

65 °C

A stirred mixture of 7-acetyl-5-fluoroquinolin-8-yltrifluoromethanesulfonate (1.00 g, 2.96 mmol, from Example 53, Step 2), piperazine (0.511 g, 5.93 mmol), and cesium carbonate (2.90 g, 8.90 mmol) in tetrahydrofuran (30 mL) was heated at 65° C. overnight. The mixture was cooled, diluted with dichloromethane and filtered. The filtrate was washed with brine, dried over sodium sulfate and evaporated to dryness. The resulting residue was purified on silica gel, eluting with 0 to 20% methanol in dichloromethane, to give the desired product (82 mg, 10%). LCMS calculated for C15H17FN3O (M+H)+: m/z=274.1; Found: 274.1.

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. washThe filtrate was washed with brine
4. dry with materialdried over sodium sulfate
5. customevaporated to dryness
6. customThe resulting residue was purified on silica gel
7. washeluting with 0 to 20% methanol in dichloromethane