Isoamyl Nitrite → 6-Fluoro-4-nitroso-3,4-dihydro-2H-benzo[1,4]oxazine

HRID 2382116Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2382116
[N:1](OCCC(C)C)=[O:2].[F:9][C:10]1[CH:11]=[CH:12][C:13]2[O:18][CH2:17][CH2:16][NH:15][C:14]=2[CH:19]=1>C(Cl)Cl>[F:9][C:10]1[CH:11]=[CH:12][C:13]2[O:18][CH2:17][CH2:16][N:15]([N:1]=[O:2])[C:14]=2[CH:19]=1

Komponenten

4

Edukt 2

HCID 8053Isoamyl NitriteHCID 162444596-Fluoro-3,4-dihydro-2H-1,4-benzoxazine

Produkt 1

HCID 866393826-Fluoro-4-nitroso-3,4-dihydro-2H-benzo[1,4]oxazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Isoamyl nitrite is added to a solution of 6-fluoro-3,4-dihydro-2H-benzo[1,4]oxazine (1 g) in DCM (15 mL) and heated to reflux overnight. The reaction mixture is concentrated in vacuo and the residue is purified by silica gel chromatography eluting with 10% EtOAc in heptane to give 6-Fluoro-4-nitroso-3,4-dihydro-2H-benzo[1,4]oxazine (0.83 g).

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux overnight
  3. concentrationThe reaction mixture is concentrated in vacuo
  4. customthe residue is purified by silica gel chromatography
  5. washeluting with 10% EtOAc in heptane

Quellen und Nachweise

ORD-Eintrag
ord-c614821056c248cf81d3702b9e6e3c91
Quelldatensatz
uspto-grants-2012_09
Patentnummer
US08258130B2

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