Nitric Acid → HCID 14771561, Verbindung

HRID 329721Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 329721
[CH3:1][N:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[C:11]([C:12]([OH:14])=[O:13])[C:6]=2[O:5][CH2:4][C:3]1=[O:15].[N+:16]([O-])([OH:18])=[O:17]>S(=O)(=O)(O)O>[CH3:1][N:2]1[C:7]2[CH:8]=[C:9]([N+:16]([O-:18])=[O:17])[CH:10]=[C:11]([C:12]([OH:14])=[O:13])[C:6]=2[O:5][CH2:4][C:3]1=[O:15]

Komponenten

4

Edukt 2

HCID 944Nitric AcidHCID 14802113HCID 14802113, Verbindung

Produkt 1

HCID 14771561HCID 14771561, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel2×

Versuchsvorschrift

To a solution of 85.5 g of 3,4-dihydro-4-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid in 222 ml of concentrated sulfuric acid with cooling to -8° C. is added dropwise with stirring a mixture of 20.7 ml of fuming nitric acid (d 1.50) and 20.7 ml of concentrated sulfuric acid at a temperature below 2° C. over about 30 minutes, and the solution further stirred under cooling. The resultant solution is poured into ice-cold water with stirring. The precipitated crystals are collected by filtration, washed with water and dried to give 99 g of 3,4-dihydro-4-methyl-6-nitro-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid, melting at 256°-259° C. with decomposition.

Aufarbeitung

  1. additionis added dropwise
  2. stirringthe solution further stirred
  3. temperatureunder cooling
  4. stirringwith stirring
  5. filtrationThe precipitated crystals are collected by filtration
  6. washwashed with water
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-1400f9909759411583e99233b5dad8fd
Quelldatensatz
uspto-grants-1990_01
Patentnummer
US04892872

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