反应详情

To a mixture of aluminum chloride (66 g, 0.50 mol) in carbon disulfide (600 mL) was added dropwise a solution of 4-(4-fluorophenyl)butyryl chloride (75.3 g, 0.37 mole) in carbon disulfide (260 mL) keeping the internal temperature below 10° C. After refluxing for 0.5 h, the reaction mixture was poured into a mixture of concentrated HCl (50 mL) and ice water (800 mL). The mixture was filtered and extracted with diethyl ether. The diethyl ether extracts were dried and concentrated in vacuo to give crude 7-fluoro-1-tetralone. Vacuum distillation gave pure 7-fluoro-1-tetralone b.p., 83° C. at 0.3 mm Hg which solidified to a white solid (94%). m.p., 62°-64° C. (lit, J. Am. Chem. Soc., 89, 386, 1967; m.p., 63.5°-65.0° C.)

1. customthe internal temperature below 10° C
2. temperatureAfter refluxing for 0.5 h
3. filtrationThe mixture was filtered
4. extractionextracted with diethyl ether
5. dry with materialThe diethyl ether extracts were dried
6. concentrationconcentrated in vacuo
7. customto give crude 7-fluoro-1-tetralone
8. distillationVacuum distillation