Water → HCID 178520452, Verbindung

HRID 967753Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 967753
C[N:2]([CH:4]=[N:5][C:6](=[O:15])[CH:7]=[CH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)C.Cl.N[OH:18].[OH-].[Na+].O>C(O)(=O)C>[OH:18][NH:2][CH:4]=[N:5][C:6](=[O:15])[CH:7]=[CH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 3745097N-[(Dimethylamino)methylene]-cinnamamide

Produkt 1

HCID 178520452HCID 178520452, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

N-[(Dimethylamino)methylene]-cinnamamide (1.0 g, 5.0 mmol) was added to a solution of hydroxylamine hydrochloride (415 mg, 6.0 mmol) in acetic acid (5 mL of 70% aqueous) and aqueous NaOH (1.2 mL, 5 M, 6.0 mmol). After stirring for 1.5 h water (5 mL) was added, and the reaction mixture was cooled to 5° C. in an ice bath. The solution was partitioned between ethyl acetate and water, and the organics were dried over Na2SO4, then concentrated in vacuo to afford N-[(hydroxyamino)methylene]-cinnamamide (850 mg, 90%). This material was carried on to the next step without further purification.

Aufarbeitung

  1. additionwas added
  2. customThe solution was partitioned between ethyl acetate and water
  3. dry with materialthe organics were dried over Na2SO4
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-8d28f91bda164931a76ed093a67b4430
Quelldatensatz
uspto-grants-2005_10
Patentnummer
US06956049B1

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