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Ethanol → 3,3'-(1,4-Phenylene)bis(2,4,5-triphenylcyclopentadienone)

HRID 1595949
ノート
印刷プレビュー

反応式

HRID 1595949 の反応式
[C:1]1([CH2:7][C:8]([CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:17]1([C:23](=O)[C:24]([C:26]2[CH:31]=[CH:30][C:29]([C:32](=O)[C:33]([C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)=O)=[CH:28][CH:27]=2)=O)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[CH2:43]([OH:45])[CH3:44].[OH-].[K+]>O>[C:29]1([C:32]2[C:33]([C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)=[C:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[C:43](=[O:45])[C:44]=2[C:12]2[CH:11]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:30]=[CH:31][C:26]([C:24]2[C:23]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[C:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[C:8](=[O:9])[C:10]=2[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)=[CH:27][CH:28]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 702EthanolHCID 75931,3-Diphenyl-2-propanoneHCID 14797Potassium Hydroxide2 回HCID 1379051,4-Bis(phenylglyoxaloyl)benzene

生成物 1

HCID 28328333,3'-(1,4-Phenylene)bis(2,4,5-triphenylcyclopentadienone)

試薬・触媒・溶媒 1

HCID 962Water
溶媒

実験手順

1,3-Diphenylacetone (1.23 g, 0.00584 mol), 1,4-bis(phenylglyoxaloyl)benzene, commercially available as Bis-PGB from Ken Seika Corporation (1.000 g, 0.00292 mol) and ethanol (50 mL) are added to a 100 mL 3-necked round bottom flask fitted with a reflux condenser/nitrogen inlet. The reaction mixture is heated to reflux and an aqueous KOH solution (0.112 g, 0.002 mol) in water (2.25 mL) is added. Additional KOH is added until the solution turns dark and stays dark. The mixture is refluxed for 45 minutes and then allowed to cool. A dark solid which precipitates is collected by filtration and analyzed by 1H-NMR, 13C-NMR, HPLC and FT-IR. All data is consistent with the formation of Compound B.

後処理

  1. customfitted with a reflux condenser/nitrogen inlet
  2. temperatureThe reaction mixture is heated
  3. temperatureto reflux
  4. temperatureThe mixture is refluxed for 45 minutes
  5. temperatureto cool
  6. customA dark solid which precipitates
  7. filtrationis collected by filtration

出典と根拠

ORDレコード
ord-85063857d93140d2a3d830d7aa231f03
出典データセット
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06288188B1

反応ノート

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