反应详情

4-Amino-6-fluoro-5-hydroxy-2-methylbiphenyl-3-carbonitrile (I-41) (1.66 g, 6.86 mmol) and di(imidazol-1-yl)methanimine (2.821 g) were suspended in tetrahydrofuran (33 ml), and stirred under reflux under nitrogen atmosphere for 120 hours. After cooling to room temperature, the solvent was evaporated away under reduced pressure. The residue was fractionated with 10% methanol-containing chloroform and water. The organic layer was separated, and dried over anhydrous sodium sulfate. The insoluble matter was separated by filtration, and the solvent was evaporated away under reduced pressure. The residue was recrystallized form methanol to obtain the entitled compound (1.60 g, 87%) as a pale brown solid.

1. temperatureunder reflux under nitrogen atmosphere for 120 hours
2. customthe solvent was evaporated away under reduced pressure
3. additioncontaining chloroform and water
4. customThe organic layer was separated
5. dry with materialdried over anhydrous sodium sulfate
6. customThe insoluble matter was separated by filtration
7. customthe solvent was evaporated away under reduced pressure
8. customThe residue was recrystallized form methanol