反应详情

Benzenethiol (500 mg, 4.537 mmol) was dissolved in 6 mL of DMF. K2CO3 (940 mg, 6.81 mmol) was then added and the resulting mixture was allowed to stir at room temperature for 10 minutes. 4-Fluorobenzaldehyde (675 mg, 5.4 mmol) was then added and the resulting mixture was allowed to stir at 50° C. for 2 hours. The mixture was then stirred at 80° C. for 3 hours. Water was then added and the product was extracted with EtOAc and washed with brine. The organic phase was dried over Na2SO4 and concentrated under reduced pressure to afford a crude product. Purification by column chromatography (using 60-120 mesh silica gel and 5:95: EtOAc:Hexane as the eluent) afforded 940 mg (96% yield) of 4-phenylsulfanyl-benzaldehyde. LC-MS purity: 91.3

1. stirringto stir at 50° C. for 2 hours
2. stirringThe mixture was then stirred at 80° C. for 3 hours
3. extractionthe product was extracted with EtOAc
4. washwashed with brine
5. dry with materialThe organic phase was dried over Na2SO4
6. concentrationconcentrated under reduced pressure
7. customto afford a crude product
8. customPurification by column chromatography (