反应详情

To a stirred solution of 4-amino-2-fluorophenol (1.27 g, 10 mmol) in 30 mL of toluene at room temperature under nitrogen in a Dean Stark apparatus was added benzaldehyde (1.01 ml, 10 mmol) followed by p-toluenesulfonic acid monohydrate (38 mg, 0.2 mmol). The mixture was heated to reflux for 4 hours. The reaction was cooled to room temperature and a solid crystallized out of the reaction mixture. The mixture was cooled to 0° C. and then filtered and the solids rinsed with toluene. The isolated tan crystals were dried under high vacuum (1.5 gm, 70% yield).

1. temperatureThe mixture was heated
2. temperatureto reflux for 4 hours
3. customa solid crystallized out of the reaction mixture
4. temperatureThe mixture was cooled to 0° C.
5. filtrationfiltered
6. washthe solids rinsed with toluene
7. customThe isolated tan crystals were dried under high vacuum (1.5 gm, 70% yield)