反応 #554600

反応方程式

2-hydroxytriphenylene

2,6-dimethylpiridine

trifluoromethanesulfonic acid anhydride

→

triphenylenyl trifluoromethanesulfonate

収率 90.0%

溶媒

methylene chloride

反応条件

後処理

1. 1
   温度while increasing temperature of the reaction solution to room temperature
2. 2
   ろ過The deposited solid was collected by filtration
3. 3
   洗浄washed with water and methanol
4. 4
   その他dried

実験手順

Under an argon atmosphere, 12.5 g of 2-hydroxytriphenylene and 0.93 g of 4-dimethylaminopiridine were placed in a flask, 200 mL of methylene chloride was added thereto and the reaction solution was cooled to −78° C. 8.22 g of 2,6-dimethylpiridine was added to the reaction solution and then, 17.3 g of trifluoromethanesulfonic acid anhydride was dropwise added thereto. The reaction solution was stirred for 5 hours while increasing temperature of the reaction solution to room temperature. The deposited solid was collected by filtration, washed with water and methanol and then dried to obtain 17.3 g (yield: 90%) of triphenylenyl trifluoromethanesulfonate.

出典