Water → 5,8-Dibromo-2,3-diphenylquinoxaline

HRID 533584

Reaktionsgleichung

Reaktionsgleichung von HRID 533584
[Br:1][C:2]1[C:3]([NH2:10])=[C:4]([NH2:9])[C:5]([Br:8])=[CH:6][CH:7]=1.[C:11]1([C:17]([C:19]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=O)=O)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.O.C(=O)(O)[O-].[Na+]>C(O)(=O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[C:4]2[C:3]=1[N:10]=[C:17]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:19]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[N:9]2

Komponenten

6

Edukt 4

HCID 962WaterHCID 8651BenzilHCID 516892Sodium BicarbonateHCID 118215323,6-Dibromobenzene-1,2-diamine

Produkt 1

HCID 224759015,8-Dibromo-2,3-diphenylquinoxaline

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

The detailed preparation procedure is as follows: 3,6-dibromo-o-phenylene diamine (1.0 g, 3.7 mmol) was added to a solution of compound benzil (0.39 g, 1.84 mmol) in acetic acid (20 mL) at 120□, then the mixture was mixed uniformly. After refluxed for 12 hours, the fluid reactant was poured into water, and neutralized with sodium bicarbonate until neutral, then extracted with chloroform and washed with saturated brine, dried over anhydrous sodium sulfate, then it was vacuum evaporated to remove the solvent, and the resulting crude product was purified by column chromatography to give a white solid, and then it was purified by recrystallization from chloroform/n-hexane to give a white solid powder. The test result is: MS (EI) m/z: 440(M+).

Aufarbeitung

  1. customThe detailed preparation procedure
  2. additionthe mixture was mixed uniformly
  3. temperatureAfter refluxed for 12 hours
  4. extractionthen extracted with chloroform
  5. washwashed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customevaporated
  8. customto remove the solvent
  9. customthe resulting crude product was purified by column chromatography
  10. customto give a white solid
  11. customit was purified by recrystallization from chloroform/n-hexane
  12. customto give a white solid powder
  13. customThe test result

Quellen und Nachweise

ORD-Eintrag
ord-036f8be6036b4223b33192d6e1f3491f
Quelldatensatz
uspto-grants-2014_10
Patentnummer
US08853348B2

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