2,6-Lutidine → Triphenylenyl trifluoromethanesulfonate

HRID 467418ノート

反応式

HRID 467418 の反応式
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]

参加物

6

反応物 3

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

生成物 1

HCID 86647724Triphenylenyl trifluoromethanesulfonate収率 90%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

反応条件

温度
-78 °C

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.

後処理

  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

出典と根拠

ORDレコード
ord-f83cdeeb17f941808b7427d4f2f47738
出典データセット
uspto-grants-2014_01
特許番号
US08623520B2

反応ノート

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