Potassium Carbonate → HCID 19708511, Verbindung

HRID 725746Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 725746
[C:1]1([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:14][C:15]1[CH:16]=[C:17]([C:22]2[CH:27]=[CH:26][C:25](I)=[C:24]([CH3:29])[CH:23]=2)[CH:18]=[CH:19][C:20]=1[I:21].C(=O)([O-])[O-].[K+].[K+]>[Cu].[N+](C1C=CC=CC=1)([O-])=O>[CH3:29][C:24]1[CH:23]=[C:22]([C:17]2[CH:18]=[CH:19][C:20]([I:21])=[C:15]([CH3:14])[CH:16]=2)[CH:27]=[CH:26][C:25]=1[N:7]([C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 11487DiphenylamineHCID 223236094,4'-Diiodo-3,3'-dimethyl-1,1'-biphenyl

Produkt 1

HCID 19708511HCID 19708511, VerbindungAusbeute 57,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23978CopperKatalysatorHCID 7416NitrobenzeneLösungsmittel

Versuchsvorschrift

20.3 g (0.12 mol) of diphenylamine, 65.1 g (0.15 mol) of 3,3'-dimethyl-4,4'-diiodobiphenyl, 19.3 g (0.14 mol) of anhydrous potassium carbonate, 1.52 g (0.024 mol) of copper powder, and 20 ml of nitrobenzene were mixed. The reaction mixture was then allowed to undergo reaction at a temperature of 190° C. to 205° C. for 21 hours. The reaction product was then extracted with 200 ml of toluene. The insoluble contents were removed by filtration. The filtrate was then concentrated to dryness. The concentrate was then purified by column chromatography (carrier: silica gel; elute: 2/7 mixture of toluene and n-hexane) to obtain 32.6 g (yield: 57.2%) of N-(3,3'-dimethyl-4'-iodo-4-biphenylyl)-N,N-diphenylamine.

Aufarbeitung

  1. customreaction at a temperature of 190° C. to 205° C. for 21 hours
  2. extractionThe reaction product was then extracted with 200 ml of toluene
  3. customThe insoluble contents were removed by filtration
  4. concentrationThe filtrate was then concentrated to dryness
  5. customThe concentrate was then purified by column chromatography (carrier: silica gel; elute: 2/7 mixture of toluene and n-hexane)

Quellen und Nachweise

ORD-Eintrag
ord-c7517e6b1b434c73acc77f86d5acd191
Quelldatensatz
uspto-grants-1998_01
Patentnummer
US05707747

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