反应详情

4-Ethynyl-1-iodo-2-methoxy-benzene (22.23 g, 86 mmol), 3-azido-6-fluoro-1,3,4,5-tetrahydro-1-benzazepin-2-one (20.87 g, 95 mmol), and sodium ascorbate (15.69 g, 86 mmol) were added to EtOH (155 mL) and DMF (155 mL). CuSO4.5H2O (10.75 g, 43.1 mmol) was added to 20 mL water and added dropwise to the stirring reaction mixture. The reaction stirred for 17 hrs at room temp. Dichloromethane was added and the organic layer was washed with 2N NaOH, dried with sodium sulfate and concentrated. Purification on silica gel (dichloromethane:methanol, 1-15%). 6-Fluoro-3-[4-(4-iodo-3-methoxy-phenyl)-1,2,3-triazol-1-yl]-1,3,4,5-tetrahydro-1-benzazepin-2-one (39.1 g) was obtained as a colorless solid and carried on the next step.

1. additionadded dropwise to the stirring reaction mixture
2. washthe organic layer was washed with 2N NaOH
3. dry with materialdried with sodium sulfate
4. concentrationconcentrated
5. customPurification on silica gel (dichloromethane:methanol, 1-15%)