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Hydroxyamine hydrochloride → HCID 73516783, Verbindung

HRID 482149
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 482149
[F:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:8]=[C:9]([C:13]3[CH2:17][CH2:16][C:15](=O)[CH:14]=3)[CH:10]=[CH:11][CH:12]=2)=[CH:4][CH:3]=1.Cl.[NH2:22][OH:23]>>[F:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:8]=[C:9]([C:13]3[CH2:17][CH2:16][C:15](=[N:22][OH:23])[CH:14]=3)[CH:10]=[CH:11][CH:12]=2)=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 2

HCID 443297Hydroxyamine hydrochlorideHCID 19065571HCID 19065571, Verbindung

Produkt 1

HCID 73516783HCID 73516783, VerbindungAusbeute 113,6 %

Versuchsvorschrift

To a stirred solution of 3-[3-(4-fluorophenoxy)phenyl]-2-cyclopentenone (10 g; 0.0373M) in ethanol-pyridine (75 ml-21 ml) was added hydroxylamine hydrochloride (3.37 g; 0.0485M) at room temperature. After stirring for 4 hrs, solvent was removed. To the residue was added dilute aqueous HCl (100 ml), and the whole was extracted with ethyl acetate (200 ml×1, 100 ml×1). The combined organic layers were washed with water (100 ml), brine (100 ml), dried over MgSO4, and concentrated in vacuo to give 12 g of crude subtitle compound [E] as a brown oil, which was used without further purification.

Aufarbeitung

  1. customsolvent was removed
  2. addition
To the residue was added dilute aqueous HCl (100 ml)
  • extractionthe whole was extracted with ethyl acetate (200 ml×1, 100 ml×1)
  • washThe combined organic layers were washed with water (100 ml), brine (100 ml)
  • dry with materialdried over MgSO4
  • concentrationconcentrated in vacuo
  • Quellen und Nachweise

    ORD-Eintrag
    ord-83e7addb87c64214b6be58776e2478cc
    Quelldatensatz
    uspto-grants-1998_08
    DOI
    10.6084/m9.figshare.5104873.v1
    Patentnummer
    US05792882

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