反应详情

温度

90 °C

A mixture of 4-bromoresorcinol (5.00 g, 26.5 mmol) and 3,3-dimethylacrylic acid (2.64 g, 26.5 mmol) were ground in a mortar. The mixture was then added portion-wise into polyphosphoric acid (8 g) at 90° C. After stirred at 90° C. for 15 min, the reaction mixture was cooled to room temperature and quenched with water. The mixture was then extracted with diethyl ether. The organic layer was separated, washed with water, brine, dried (MgSO4) and concentrated at reduced pressure to give a yellow residue. Purification by recrystallization (methanol and water) afforded the title compound as a yellow solid.

1. temperaturethe reaction mixture was cooled to room temperature
2. customquenched with water
3. extractionThe mixture was then extracted with diethyl ether
4. customThe organic layer was separated
5. washwashed with water, brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated at reduced pressure
8. customto give a yellow residue
9. customPurification
10. customby recrystallization (methanol and water)