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

HRID 703400
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HRID 703400 반응식
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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 23978Copper촉매

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온도
150 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-367e8f88bdd0403fb702df7298c72ca5
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04983482

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