1-Iodo-4-[(2-methylbut-3-yn-2-yl)oxy]benzene → HCID 10913124, Verbindung

HRID 1165195Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1165195
[CH3:1][C:2]([O:6][C:7]1[CH:12]=[CH:11][C:10]([I:13])=[CH:9][CH:8]=1)([CH3:5])[C:3]#[CH:4]>N1C2C(=CC=CC=2)C=CC=1.CCOCC>[CH3:5][C:2]1([CH3:1])[CH:3]=[CH:4][C:8]2[CH:9]=[C:10]([I:13])[CH:11]=[CH:12][C:7]=2[O:6]1

Komponenten

4

Edukt 1

HCID 149335571-Iodo-4-[(2-methylbut-3-yn-2-yl)oxy]benzene

Produkt 1

HCID 10913124HCID 10913124, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 7047QuinolineLösungsmittel

Versuchsvorschrift

A solution of 1-[(1,1-dimethyl-2-propynyl)oxy]-4-iodobenzene (5.97 g, 20.8 mmol) in quinoline (25 mL) was heated at 170° C. for 2 hours. The reaction was cooled to room temperature and diluted with ether. The reaction mixture was washed with 2N HCl (4X eq. vol.), with brine (2X eq. vol.), dried over anhydrous MgSO4 and concentrated to give crude product. This material was combined with product from an identical reaction and purified by flash chromatography, using 100% petroleum ether elution to give 5.58 g, (79% for the two reactions), of product.

Aufarbeitung

  1. washThe reaction mixture was washed with 2N HCl (4X eq. vol.), with brine (2X eq. vol.)
  2. dry with materialdried over anhydrous MgSO4
  3. concentrationconcentrated
  4. customto give crude product
  5. customThis material was combined with product from an identical reaction
  6. custompurified by flash chromatography
  7. wash100% petroleum ether elution
  8. customto give 5.58 g

Quellen und Nachweise

ORD-Eintrag
ord-e496ebf3374341c9b30e48e82aa15b71
Quelldatensatz
uspto-grants-1990_03
Patentnummer
US04908378

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