Water → 2-methyl-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazine-6-carbaldehyde

HRID 840374Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 840374
C([O:3][C:4](=O)[CH:5]([O:7][C:8]1[CH:13]=[CH:12][C:11]([CH:14]2OCC[O:15]2)=[CH:10][C:9]=1[N+:19]([O-])=O)[CH3:6])C.O>C(O)(=O)C.[Fe]>[CH:14]([C:11]1[CH:12]=[CH:13][C:8]2[O:7][CH:5]([CH3:6])[C:4](=[O:3])[NH:19][C:9]=2[CH:10]=1)=[O:15]

Komponenten

5

Edukt 2

HCID 962Water2×HCID 57232269HCID 57232269, Verbindung

Produkt 1

HCID 218738872-methyl-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazine-6-carbaldehydeAusbeute 97,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

28.8 g of pulverized iron is added in portions to 34 g of 2-(4-(1,3-dioxolan-2-yl)-2-nitrophenoxy)propionic acid ethyl ester in 360 ml of glacial acetic acid with 80 ml of water while being cooled in an ice bath. The mixture is hot. After 2 hours, it is poured onto 1 l of water, extracted with ethyl acetate, and the organic phase is washed with brine. It is dried with magnesium sulfate and concentrated by evaporation. 20.3 g of brownish solid results.

Aufarbeitung

  1. temperaturewhile being cooled in an ice bath
  2. extractionextracted with ethyl acetate
  3. washthe organic phase is washed with brine
  4. dry with materialIt is dried with magnesium sulfate
  5. concentrationconcentrated by evaporation

Quellen und Nachweise

ORD-Eintrag
ord-ed45fd133e4c4bba840060cc69578bfd
Quelldatensatz
uspto-grants-2002_04
Patentnummer
US06365736B1

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