反应详情

A solution of 44 ml of 4-bromo-1-fluorobenzene in 300 ml of anhydrous diethyl ether is added dropwise to a suspension of 9.6 g of magnesium turnings in 20 ml of anhydrous diethyl ether. When the addition is complete, the mixture is stirred for a few minutes at room temperature and a solution of 46 g of 4-benzylthiobenzonitrile, prepared in Example 55, in 400 ml of anhydrous tetrahydrofuran is added dropwise. The diethyl ether is distilled and the mixture is refluxed for 3 hours and then cooled with ice. 6N hydrochloric acid solution (400 ml) is added dropwise and the mixture is refluxed for 6 hours. After the addition of water and dichloromethane, the organic phase is decanted, dried over magnesium sulfate and then evaporated under vacuum. The residue crystallizes from diisopropyl ether to give 48 g of 4-benzylthio-4'-fluorobenzophenone in the form of crystals melting at 96° C.

1. additionWhen the addition
2. additionis added dropwise
3. distillationThe diethyl ether is distilled
4. temperaturethe mixture is refluxed for 3 hours
5. temperaturecooled with ice
6. addition6N hydrochloric acid solution (400 ml) is added dropwise
7. temperaturethe mixture is refluxed for 6 hours
8. additionAfter the addition of water and dichloromethane
9. customthe organic phase is decanted
10. dry with materialdried over magnesium sulfate
11. customevaporated under vacuum
12. customThe residue crystallizes from diisopropyl ether