Hydroxyamine hydrochloride → HCID 73508098, Verbindung

HRID 2259651Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2259651
OC1[O:6][CH:5]([C:7]2[S:8][C:9]3[CH:15]=[C:14]([N:16]4[CH2:20][CH:19]([CH2:21][O:22][CH3:23])[O:18][C:17]4=[O:24])[CH:13]=[CH:12][C:10]=3[N:11]=2)[CH2:4][CH2:3]1.Cl.[NH2:26][OH:27]>N1C=CC=CC=1>[OH:6][CH:5]([C:7]1[S:8][C:9]2[CH:15]=[C:14]([N:16]3[CH2:20][CH:19]([CH2:21][O:22][CH3:23])[O:18][C:17]3=[O:24])[CH:13]=[CH:12][C:10]=2[N:11]=1)[CH2:4][CH:3]=[N:26][OH:27]

Komponenten

4

Edukt 2

HCID 443297Hydroxyamine hydrochlorideHCID 15342529HCID 15342529, Verbindung

Produkt 1

HCID 73508098HCID 73508098, VerbindungAusbeute 101,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

72 g of the 3-[2-(5-hydroxytetrahydrofuran-2-yl)-benzothiazol-6-yl]-5-methoxymethyl-2-oxazolidinone obtained in the Example 7 was dissolved in 150 ml of pyridine. 18.6 g of hydroxylamine hydrochloride was added to the solution at room temperature and the mixture was stirred for 10 min and then poured into ice/water. After extraction with ethyl acetate followed by washing with dilute hydrochloric acid, an aqueous sodium hydrogencarbonate solution and an aqueous common salt solution, the product was dried over magnesium sulfate. After concentration under reduced pressure, the obtained solid was recrystallized from acetone/diisopropyl ether to give 73 g of the titled compound.

Aufarbeitung

  1. extractionAfter extraction with ethyl acetate
  2. washby washing with dilute hydrochloric acid
  3. dry with materialan aqueous sodium hydrogencarbonate solution and an aqueous common salt solution, the product was dried over magnesium sulfate
  4. concentrationAfter concentration under reduced pressure
  5. customthe obtained solid was recrystallized from acetone/diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-98c84408806d4feeb0670a114455b46e
Quelldatensatz
uspto-grants-1995_12
Patentnummer
US05475014

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