反応 #2501397

反応方程式

Di-(2-thienyl)sulfide

diphenyliodonium triflate

ethyl ether

→

title compound

収率 78.0%

di-(2-thienyl)phenylsulfonium triflate

収率 78.0%

溶媒

water

反応条件

後処理

1. 1
   温度After cooling down
2. 2
   その他the mixture vigorously stirred overnight
3. 3
   ろ過Filtration
4. 4
   洗浄washing with ethyl ether
5. 5
   その他yielded a brown solid, which
6. 6
   ろ過the solution filtered
7. 7
   その他the water removed in vacuo
8. 8
   ろ過the mixture filtered
9. 9
   洗浄the residue washed with ethyl ether

実験手順

Di-(2-thienyl)sulfide (2.1 g, 0.0104 mole), diphenyliodonium triflate (5.8 g, 0.0135 mole) and copper benzoate (0.08 g, 0.003 mole) are heated without solvent for 3 hours at 120-145° C. under a nitrogen atmosphere. After cooling down, 75 ml ethyl ether was added and the mixture vigorously stirred overnight to achieve solidification. Filtration and washing with ethyl ether yielded a brown solid, which was dissolved in hot water, the solution filtered and the water removed in vacuo. The resulting white solid was stirred in 50 ml ethyl ether for 24 hours, the mixture filtered and the residue washed with ethyl ether, yielding 3.4 g (78%) of the title compound, di(2-thienyl)phenylsulfonium triflate. The structure was confirmed by 1H/13C NMR spectroscopy.

出典