反应详情

To 10 g of 5-fluoro-2-[(3-fluorophenyloxy)methyl]benzoic acid is added 50 g of thionyl chloride and the mixture is refluxed with heating for 1 hour. After cooling the reaction mixture to room temperature, dry toluene is added and the solvent is distilled off under reduced pressure. The residue is added with dichloromethane and cooled to 0° C. Thereto 10 g of powdery anhydrous aluminum chloride is added and the mixture is stirred for 15 minutes. The reaction mixture is added with ice-water and extracted with toluene. After the extract is dried over magnesium fulfate, the solvent is distilled off under reduced pressure and the residue is subjected to silica-gel chromatography, followed by elution with toluene to give 4.3 g of 3,9-difluoro-6,11-dihydrodibenz[b,e]oxepin-11-one (oil). Mass spectrum m/z: 246(M+).

1. temperaturethe mixture is refluxed
2. temperaturewith heating for 1 hour
3. distillationthe solvent is distilled off under reduced pressure
4. additionThe residue is added with dichloromethane
5. temperaturecooled to 0° C
6. additionThereto 10 g of powdery anhydrous aluminum chloride is added
7. additionThe reaction mixture is added with ice-water
8. extractionextracted with toluene
9. dry with materialAfter the extract is dried over magnesium fulfate
10. distillationthe solvent is distilled off under reduced pressure
11. washfollowed by elution with toluene