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Potassium Carbonate → 2,7-Bis(phenyl-m-tolylamino)-9,9-bis[2-(methoxycarbonyl)ethyl]fluorene

HRID 703400
ノート
印刷プレビュー

反応式

HRID 703400 の反応式
I[C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8](I)=[CH:9][CH:10]=3)[C:5]([CH2:22][CH2:23][C:24]([O:26][CH3:27])=[O:25])([CH2:16][CH2:17][C:18]([O:20][CH3:21])=[O:19])[C:4]=2[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[C:34]1([NH:40][C:41]2[CH:46]=[CH:45][CH:44]=[C:43]([CH3:47])[CH:42]=2)[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1>[Cu]>[C:34]1([N:40]([C:41]2[CH:42]=[C:43]([CH3:47])[CH:44]=[CH:45][CH:46]=2)[C:2]2[CH:14]=[CH:13][C:12]3[C:11]4[C:6](=[CH:7][C:8]([N:40]([C:34]5[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=5)[C:41]5[CH:42]=[C:43]([CH3:47])[CH:44]=[CH:45][CH:46]=5)=[CH:9][CH:10]=4)[C:5]([CH2:22][CH2:23][C:24]([O:26][CH3:27])=[O:25])([CH2:16][CH2:17][C:18]([O:20][CH3:21])=[O:19])[C:4]=3[CH:3]=2)[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 14569N-(3-Methylphenyl)anilineHCID 198174132,7-Diiodo-9,9-bis[2-(methoxycarbonyl)ethyl]fluorene

生成物 1

HCID 145978792,7-Bis(phenyl-m-tolylamino)-9,9-bis[2-(methoxycarbonyl)ethyl]fluorene

試薬・触媒・溶媒 1

HCID 23978Copper触媒

反応条件

温度
150 °C

実験手順

A mixture of 17.0 grams of 2,7-diiodo-9,9-bis[2-(methoxycarbonyl)ethyl]fluorene, 4.3 grams of copper bronze, 12.5 grams of potassium carbonate in 30 milliliters of Soltrol 220 was mechanically stirred and heated to 150° C. under a nitrogen atmosphere. Fifteen (15.0) grams of molten N-phenyl-m-toluidine was added dropwise at this temperature. After addition, the resulting mixture was heated at 210° C. under reflux for 24 hours. The hot reaction mixture was filtered, and the filter cake was washed several times with hot cyclohexane. The combined filtrate was evaporated under reduced pressure to give a brown residue which was purified by column chromatography on silica gel to afford 15.2 grams of pure 2,7-bis(phenyl-m-tolylamino)-9,9-bis[2-(methoxycarbonyl)ethyl]-fluorene, melting point 159° to 160° C.

後処理

  1. additionAfter addition
  2. temperaturethe resulting mixture was heated at 210° C.
  3. temperatureunder reflux for 24 hours
  4. filtrationThe hot reaction mixture was filtered
  5. washthe filter cake was washed several times with hot cyclohexane
  6. customThe combined filtrate was evaporated under reduced pressure
  7. customto give a brown residue which
  8. customwas purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-367e8f88bdd0403fb702df7298c72ca5
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04983482

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート