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Sulfuric acid magnesium salt (1:1) → 2-[4-(Benzyloxy)-3-bromobenzyl]azulene

HRID 1375988
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1375988
N1[CH2:5][CH2:4][CH2:3][CH2:2]1.S([O-])([O-])(=O)=O.[Mg+2].[CH2:12]([O:19][C:20]1[CH:25]=[CH:24][C:23]([CH2:26][C:27]([CH3:29])=O)=[CH:22][C:21]=1[Br:30])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(OCC)C>[CH2:12]([O:19][C:20]1[CH:25]=[CH:24][C:23]([CH2:26][C:27]2[CH:5]=[C:4]3[C:2](=[CH:3][CH:4]=[CH:5][CH:2]=[CH:3]3)[CH:29]=2)=[CH:22][C:21]=1[Br:30])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 31268PyrrolidineHCID 230805631-[3-Bromo-4-(phenylmethoxy)phenyl]-2-propanone

Produkt 1

HCID 587861482-[4-(Benzyloxy)-3-bromobenzyl]azulene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

Pyrrolidine (1.9 ml) and magnesium sulfate (2.74 g) were added to a solution of 1-[4-(benzyloxy)-3-bromophenyl]acetone (3.65 g) in diethyl ether (30 ml) and the mixture was stirred at room temperature for 12 hours. After filtration, the solvent was evaporated under reduced pressure. The resulting residue was dried under reduced pressure and dissolved in ethanol (30 ml). 2H-cyclohepta[b]furan-2-on (0.5 g) was added to the solution and the mixture was refluxed with heating for eight hours. The reaction mixture was concentrated. The resulting residue was purified by silica gel column chromatography (ethyl acetate-n-hexane) to obtain 2-[4-(benzyloxy)-3-bromobenzyl]azulene (0.84 g).

Aufarbeitung

  1. filtrationAfter filtration
  2. customthe solvent was evaporated under reduced pressure
  3. customThe resulting residue was dried under reduced pressure
  4. dissolutiondissolved in ethanol (30 ml)
  5. addition2H-cyclohepta[b]furan-2-on (0.5 g) was added to the solution
  6. temperaturethe mixture was refluxed
  7. temperaturewith heating for eight hours
  8. concentrationThe reaction mixture was concentrated
  9. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate-n-hexane)

Quellen und Nachweise

ORD-Eintrag
ord-05f313adf1594475af3041ceb4cb81e2
Quelldatensatz
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07169761B2

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