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1,3,5-Trimethoxy-4-iodobenzene → 1,3,5-Trimethoxy-2-(2,4,6-trimethoxyphenyl)benzene

HRID 919185
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 919185
I[C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([O:10][CH3:11])=[CH:4][C:3]=1[O:12][CH3:13]>[Cu]>[CH3:13][O:12][C:3]1[CH:4]=[C:5]([O:10][CH3:11])[CH:6]=[C:7]([O:8][CH3:9])[C:2]=1[C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([O:10][CH3:11])=[CH:4][C:3]=1[O:12][CH3:13]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 122540971,3,5-Trimethoxy-4-iodobenzene

Produkt 1

HCID 52193411,3,5-Trimethoxy-2-(2,4,6-trimethoxyphenyl)benzeneAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 23978CopperKatalysator

Reaktionsbedingungen

Temperatur
235 °C

Versuchsvorschrift

Compound 6 (7.0 g, 0.024 mol) and copper powder (2.0 g, 0.03 1 mol) were mixed thoroughly and transferred to a heavy wall, pressure vessel. The vessel was placed into a sand-bath at the initial temperature of 120° C. Once the vessel was secured, the temperature of the bath was raised to 235° C. in 15 min and kept at 235° C. for 1 h. The vessel was allowed to cool and the contents removed and powdered. The product was extracted with methanol for 18 h in a soxhlet. The resultant solution was concentrated in vacuo. Purification of the crude reaction mixture via column chromatography (1:5 ethyl acetate/hexane) yielded 7 (3.1 g, 78%) as a white solid.

Aufarbeitung

  1. customThe vessel was placed into a sand-bath
  2. customtemperature of 120° C
  3. temperatureto cool
  4. customthe contents removed
  5. extractionThe product was extracted with methanol for 18 h in a soxhlet
  6. concentrationThe resultant solution was concentrated in vacuo
  7. customPurification of the crude
  8. customreaction mixture via column chromatography (1:5 ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-17feb5d680ca47cd86bd7b1a674c0883
Quelldatensatz
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09273021B2

Notizen zur Reaktion

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