Bromide ion → HCID 13627996, Verbindung

HRID 1981477

Reaktionsgleichung

Reaktionsgleichung von HRID 1981477
Br[C:2]1[C:3](Br)=[C:4](Br)[C:5](Br)=[C:6]([CH3:9])[C:7]=1[CH3:8].[I-].[K+].[CH3:15][O:16][C:17]1[C:18](=[O:24])[CH:19]=[CH:20][C:21](=[O:23])[CH:22]=1.[Br-]>CN(C)C=O.O>[CH3:15][O:16][C:17]1[C:18](=[O:24])[C:19]2[C:20]([C:21](=[O:23])[CH:22]=1)=[CH:8][C:7]1[C:6](=[CH:5][CH:4]=[CH:3][CH:2]=1)[CH:9]=2

Komponenten

7

Edukt 4

HCID 259Bromide ionHCID 4875Potassium IodideHCID 177713,4,5,6-Tetrabromo-o-xyleneHCID 761462-Methoxy-1,4-benzoquinone

Produkt 1

HCID 13627996HCID 13627996, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

16 g of, α, α, α', α', -tetrabromo-o-xylene, 44 g of potassium iodide and 10 g crude 2-methoxy-1,4-benzoquinone were stirred in 160 ml of N,N-dimethylformamide at 70° C. overnight. After the reaction was complete, no bromide was left as determined by thin layer chromotography and the reaction mixture was poured into 1200 ml of H2O. 10%aq Na2S2O5 solution was added to decolorize the solution. The precipitate formed in the aqueous solution was collected and dried. Continuous extraction of the dark precipitate using benzene as a solvent yielded a dark colored solution. The solution was then washed with 2.5% NaOH, H2O, dried and concentrated. 7 g of crude product was obtained. Recrystallization from methanol yielded 5 g of pure yellow powder of MAQ.

Aufarbeitung

  1. customThe precipitate formed in the aqueous solution
  2. customwas collected
  3. customdried
  4. extractionContinuous extraction of the dark precipitate
  5. customyielded a dark colored solution
  6. washThe solution was then washed with 2.5% NaOH, H2O
  7. customdried
  8. concentrationconcentrated
  9. custom7 g of crude product was obtained
  10. customRecrystallization from methanol

Quellen und Nachweise

ORD-Eintrag
ord-a0ae162123864df5a17da0e2bc6f7314
Quelldatensatz
uspto-grants-1986_06
Patentnummer
US04592867

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