2,6-Lutidine → Triphenylenyl trifluoromethanesulfonate

HRID 467418노트

반응식

HRID 467418 반응식
O[C:2]1[CH:19]=[CH:18][C:17]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[C:4]=2[CH:3]=1.CC1C=CC=C(C)N=1.[F:28][C:29]([F:42])([F:41])[S:30]([O:33]S(C(F)(F)F)(=O)=O)(=[O:32])=[O:31]>CN(C)C1C=CN=CC=1.C(Cl)Cl>[F:28][C:29]([F:42])([F:41])[S:30]([O:33][C:3]1[C:4]2[C:5]3[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=3)[C:11]3[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:17]=2[CH:18]=[CH:19][CH:2]=1)(=[O:32])=[O:31]

참가 물질

6

반응물 3

HCID 79372,6-LutidineHCID 67749Trifluoromethanesulfonic anhydrideHCID 3016112Triphenylen-2-ol

생성물 1

HCID 86647724Triphenylenyl trifluoromethanesulfonate수율 90%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

반응 조건

온도
-78 °C

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.

후처리

  1. temperaturewhile increasing temperature of the reaction solution to room temperature
  2. filtrationThe deposited solid was collected by filtration
  3. washwashed with water and methanol
  4. customdried

출처 및 근거

ORD 기록
ord-f83cdeeb17f941808b7427d4f2f47738
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08623520B2

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