反应详情

温度

75 °C

To a solution of methyl 4-(cyanomethyl)-3-fluorobenzoate (8 g, 41 mmol) and resorcinol (6.8 g, 62 mmol) in BF3-Et2O (100 ml) was bubbled with HCl at 0° C. for 15 min. The mixture was stirred at 75° C. for 16 hours. Then H2O (100 ml) was added and the solution was heated at 95° C. for 16 hours. The mixture was cooled to room temperature and neutralized by Na2CO3 and extracted with EtOAc (100 ml×3). The organic layers were combined, dried with anhydrous Na2SO4, filtered and evaporated to give the crude product. Purification by column chromatography (PE/EtOAc=10/1 to 3/1) gave Intermediate I as a white solid (6 g, 48%).

1. temperaturethe solution was heated at 95° C. for 16 hours
2. temperatureThe mixture was cooled to room temperature
3. extractionextracted with EtOAc (100 ml×3)
4. dry with materialdried with anhydrous Na2SO4
5. filtrationfiltered
6. customevaporated
7. customto give the crude product
8. customPurification by column chromatography (PE/EtOAc=10/1 to 3/1)