N-bromobutanimide → HCID 23298010, Verbindung

HRID 1422210Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1422210
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[N:9]2)=[C:4]([CH3:16])[CH:3]=1.[Br:17]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[N:9]2)=[C:4]([CH2:16][Br:17])[CH:3]=1

Komponenten

4

Edukt 2

HCID 67184N-bromobutanimideHCID 232980507-Bromo-5-methyl-2,3-dimethoxy-quinoxaline

Produkt 1

HCID 23298010HCID 23298010, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5943Carbon TetrachlorideLösungsmittel

Versuchsvorschrift

15 g (53 mmol) of 7-bromo-5-methyl-2,3-dimethoxy-quinoxaline, 9.9 g (1.05 equiv.) of N-bromosuccinimide and 0.87 g (0.1 equiv.) of azo-isobutyronitrile are dissolved in 100 ml of carbon tetrachloride and the solution is stirred at reflux for 24 hours. The solid is filtered off and the filtrate is diluted with dichloromethane, then washed once with each of water and brine. The organic phase is dried over magnesium sulfate and concentrated by evaporation. The residue is recrystallized from ethyl acetate and hexane. The title compound is obtained in the form of light-orange crystals.

Aufarbeitung

  1. temperatureat reflux for 24 hours
  2. filtrationThe solid is filtered off
  3. additionthe filtrate is diluted with dichloromethane
  4. washwashed once with each of water and brine
  5. dry with materialThe organic phase is dried over magnesium sulfate
  6. concentrationconcentrated by evaporation
  7. customThe residue is recrystallized from ethyl acetate and hexane

Quellen und Nachweise

ORD-Eintrag
ord-94c68e858ea046f886de8dc83e034cfe
Quelldatensatz
uspto-grants-2000_06
Patentnummer
US06080743

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