Dimethylformamide → HCID 86755366, Verbindung

HRID 1106879Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1106879
[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[OH:11].[Br:12][CH2:13][CH2:14]Br.CN(C)C=O.C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C.O>[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[O:11][CH2:14][CH2:13][Br:12]

Komponenten

7

Edukt 4

HCID 6228DimethylformamideHCID 78391,2-DibromoethaneHCID 11430Potassium CarbonateHCID 221092-Bromo-4-nitrophenol

Produkt 1

HCID 86755366HCID 86755366, VerbindungAusbeute 62,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
82.5 °C

Versuchsvorschrift

A portion (2.3 g, 10.6 mmol) of the 2-bromo-4-nitrophenol produced in (1) above and 1,2-dibromoethane (7.9 g, 42.1 mmol) were added to N,N-dimethylformamide (20 ml); to the mixture, potassium carbonate (1.6 g) was added, followed by stirring at 80-85° C. for 3 h. The reaction mixture was added to water (100 ml) and extraction was conducted with ethyl acetate, followed by the drying of the extract with magnesium sulfate and concentration. The residue was subjected to column chromatography using a 10:3:1 solvent system of n-hexane, ethyl ether and ethyl acetate as an eluent to yield the end compound 1-(2-bromo-4-nitrophenoxy-2-bromoethane (2.14 g).

Aufarbeitung

  1. customdrying of the
  2. extractionextract with magnesium sulfate and concentration

Quellen und Nachweise

ORD-Eintrag
ord-6857e1eefdbc4824b96790698ff4583c
Quelldatensatz
uspto-grants-2000_05
Patentnummer
US06057358

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