反应详情

To a suspension of 9.6 g of magnesium turnings in 20 ml of anhydrous diethyl ether is added dropwise a solution of 44 ml of 4-bromo-1-fluorobenzene in 300 ml of anhydrous diethyl ether. At the end of the addition, the mixture is stirred for a few minutes at room temperature and a solution of 46 g of 4-benzylthiobenzonitrile, prepared in example 16, in 400 ml of anhydrous tetrahydrofuran is added dropwise. The diethyl ether is distilled off and the mixture is heated under reflux for 3 hours before being cooled with ice. A 6M solution of hydrochloric acid (400 ml) is added dropwise and the mixture is heated under reflux for 6 hours. After the addition of water and dichloromethane, the organic phase is separated, dried over magnesium sulfate and evaporated in vacuo. The residue crystallizes in diisopropyl ether to give 48 g of 4-benzylthio-4'-fluorobenzophenone as crystals with a melting point of 96° C.

1. additionAt the end of the addition
2. additionis added dropwise
3. distillationThe diethyl ether is distilled off
4. temperaturethe mixture is heated
5. temperatureunder reflux for 3 hours
6. temperaturebefore being cooled with ice
7. additionA 6M solution of hydrochloric acid (400 ml) is added dropwise
8. temperaturethe mixture is heated
9. temperatureunder reflux for 6 hours
10. additionAfter the addition of water and dichloromethane
11. customthe organic phase is separated
12. dry with materialdried over magnesium sulfate
13. customevaporated in vacuo
14. customThe residue crystallizes in diisopropyl ether