Ammonia → 4-Bromo-5-aminophthalide

HRID 430466

Reaktionsgleichung

[Br:1][C:2]1[C:11]([N+:12]([O-])=O)=[CH:10][CH:9]=[C:8]2[C:3]=1[CH2:4][O:5][C:6]2=[O:7].O.N>C(O)C.S([O-])([O-])(=O)=O.[Fe+2]>[Br:1][C:2]1[C:11]([NH2:12])=[CH:10][CH:9]=[C:8]2[C:3]=1[CH2:4][O:5][C:6]2=[O:7]

Komponenten

Reaktionsbedingungen

Temperatur: 60 °C

Versuchsvorschrift

6.6 g of 4-bromo-5-nitrophthalide is dissolved in 45 ml of ethanol and added in drops to a mixture of 65 g of iron(II) sulfate, 220 ml of water and 65 ml of ammonia (33%) that is heated to 60° C. and thoroughly stirred. After 2 hours at 60° C., the mixture is absorptively precipitated five times with 200 ml of diethyl ether. The diethyl ether phases are concentrated by evaporation. As a residue, 4.1 g of 4-bromo-5-aminophthalide is obtained, flash point 176-180° C.

Aufarbeitung

customthe mixture is absorptively precipitated five times with 200 ml of diethyl ether
concentrationThe diethyl ether phases are concentrated by evaporation

Quellen und Nachweise

ORD-Eintrag: ord-01241adb8b4647fabe5ad1922a7e6b1c
Quelldatensatz: uspto-grants-2001_11
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06323199B1

Verknüpfte Notizen

Wird geladen…