반응 #554600

ord-f83cdeeb17f941808b7427d4f2f47738

반응 방정식

Oc1ccc2c3ccccc3c3ccccc3c2c1
2-hydroxytriphenylene
Cc1cccc(C)n1
2,6-dimethylpiridine
O=S(=O)(OS(=O)(=O)C(F)(F)F)C(F)(F)F
trifluoromethanesulfonic acid anhydride
O=S(=O)(Oc1cccc2c3ccccc3c3ccccc3c12)C(F)(F)F
triphenylenyl trifluoromethanesulfonate
수율 90.0%

반응 조건

온도
-78°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while increasing temperature of the reaction solution to room temperature
  2. 2
    여과The deposited solid was collected by filtration
  3. 3
    세척washed with water and methanol
  4. 4
    기타dried

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08623520B2uspto-grants-2014_01