反应详情

温度

150 °C

To a 250 mL round-bottomed flask fitted with a magnetic stirrer, a condenser and a nitrogen atmosphere are charged 7.85 g (0.0206 mol) of the product of Example 2, 13.5 g (0.123 mol) of resorcinol, 4 mL of m-xylene and 0.954 g (7.16 mmol) of aluminum chloride. The mixture is heated to 150° C. for 13.5 hours and then allowed to cool to 90° C. Portions of 2N hydrochloric acid and heptane are added and the mixture is stirred at 90° C. for 30 minutes followed by stirring for 18 hours at room temperature. The mixture is then warmed to 35° C. The crude solid formed is collected by vacuum filtration and is washed with portions of water and heptane. The solid is then recrystallized twice from methanol to afford 4.76 g (62% yield) of the title compound as a yellow solid melting at 194-196° C.

1. customTo a 250 mL round-bottomed flask fitted with a magnetic stirrer, a condenser
2. temperatureto cool to 90° C
3. stirringby stirring for 18 hours at room temperature
4. temperatureThe mixture is then warmed to 35° C
5. customThe crude solid formed
6. filtrationis collected by vacuum filtration
7. washis washed with portions of water and heptane
8. customThe solid is then recrystallized twice from methanol