反应详情

A mixture of 69 g (0.303 mole) of 2-mercaptobenzophenone, 82 g (0.303 mole) of mesylate 55, 32 g of triethylamine, and 150 ml of diglyme was stirred and held at reflux for 24 h. The mixture was cooled, poured into dil. HCl and extracted with methylene chloride. The organic layer was washed with 10% NaOH, water, brine, and dried over sodium sulfate and concentrated under vacuum to remove excess diglyme. This was purified by silica gel flush column (5% EtOAc:Hexane) and gave 18.6 g (75.9%) of yellow oil. Proton NMR and mass spectra were consistent with the product.

1. temperatureat reflux for 24 h
2. temperatureThe mixture was cooled
3. extractionextracted with methylene chloride
4. washThe organic layer was washed with 10% NaOH, water, brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated under vacuum
7. customto remove excess diglyme
8. customThis was purified by silica gel
9. customflush column (5% EtOAc:Hexane)