Potassium Nitrate → 7-nitro-3,4-dihydro-1,4-benzoxazepin-5(2H)-one

HRID 2296611Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2296611
[O:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5](=[O:12])[NH:4][CH2:3][CH2:2]1.[N+:13]([O-])([O-:15])=[O:14].[K+]>S(=O)(=O)(O)O>[N+:13]([C:10]1[CH:9]=[CH:8][C:7]2[O:1][CH2:2][CH2:3][NH:4][C:5](=[O:12])[C:6]=2[CH:11]=1)([O-:15])=[O:14]

Komponenten

4

Edukt 2

HCID 24434Potassium NitrateHCID 3406292,3,4,5-Tetrahydro-1,4-benzoxazepin-5-one

Produkt 1

HCID 183874717-nitro-3,4-dihydro-1,4-benzoxazepin-5(2H)-oneAusbeute 22,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To 2,3,4,5-tetrahydro-1,4-benzoxazepin-5-one (30.34 g, 190 mmol) in conc. sulfuric acid (600 ml) at 0° C. was added potassium nitrate (20.82 g, 206 mmol) portionwise. The mixture was stirred for 20 minutes at 0° C. and then for 4 h at room temperature. The mixture was poured onto ice (21) and the solids were collected by filtration. The solids were taken up in hot ethyl acetate and then cooled to yield the title compound (8.79 g, 22%), MS m/z 209 [M+H]+.

Aufarbeitung

  1. waitfor 4 h at room temperature
  2. filtrationthe solids were collected by filtration
  3. temperaturecooled

Quellen und Nachweise

ORD-Eintrag
ord-276c6523d4da4a44ad8656769ae49554
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06489322B1

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