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2,5-Bis(2,5-dimethylbenzyl)terephthalic acid → 7,14-Dihydro-1,4,8,11-tetramethylpentacene-5,12-dione

HRID 488967
ノート
印刷プレビュー

反応式

HRID 488967 の反応式
[CH3:1][C:2]1[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][C:3]=1[CH2:4][C:5]1[CH:13]=[C:12]([C:14](O)=[O:15])[C:11]([CH2:17][C:18]2[CH:23]=[C:22]([CH3:24])[CH:21]=[CH:20][C:19]=2[CH3:25])=[CH:10][C:6]=1[C:7](O)=[O:8]>FC(F)(F)S(O)(=O)=O>[CH3:1][C:2]1[C:3]2[CH2:4][C:5]3[C:6](=[CH:10][C:11]4[CH2:17][C:18]5[C:23]([C:14](=[O:15])[C:12]=4[CH:13]=3)=[C:22]([CH3:24])[CH:21]=[CH:20][C:19]=5[CH3:25])[C:7](=[O:8])[C:26]=2[C:27]([CH3:30])=[CH:28][CH:29]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 222694722,5-Bis(2,5-dimethylbenzyl)terephthalic acid

生成物 1

HCID 222694677,14-Dihydro-1,4,8,11-tetramethylpentacene-5,12-dione

試薬・触媒・溶媒 1

HCID 62406Trifluoromethanesulfonic acid溶媒

実験手順

To 200 mL of trifluoromethanesulfonic acid cooled to 18° C. was added slowly 53 grams of 2,5-bis(2,5-dimethylbenzyl)terephthalic acid in small portions as a solid at a rate such that the temperature remained below 25° C. The mixture was allowed to stir for 10 minutes and the cooling bath was removed. The mixture was stirred overnight at room temperature. The mixture was poured over 600 grams of ice and the resulting solid was collected by filtration. The solid was washed with 1 L of water followed by 500 mL of saturated aqueous sodium bicarbonate solution. The solid was washed with water until the pH of the filtrate was neutral to pH paper. The solid was stirred for one hour with 500 mL of tetrahydrofuran and collected by filtration. The solid was washed with tetrahydrofuran and dried to give 7,14-dihydro-1,4,8,11-tetramethylpentacene-5,12-dione.

後処理

  1. customremained below 25° C
  2. customthe cooling bath was removed
  3. stirringThe mixture was stirred overnight at room temperature
  4. additionThe mixture was poured over 600 grams of ice
  5. filtrationthe resulting solid was collected by filtration
  6. washThe solid was washed with 1 L of water
  7. washThe solid was washed with water until the pH of the filtrate
  8. stirringThe solid was stirred for one hour with 500 mL of tetrahydrofuran
  9. filtrationcollected by filtration
  10. washThe solid was washed with tetrahydrofuran
  11. customdried

出典と根拠

ORDレコード
ord-48cc41e466bb4b7cbd4c9a22ccf06362
出典データセット
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06974877B2

反応ノート

読み込み中…

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