Bromide ion → HCID 135458024, Verbindung

HRID 229731

Reaktionsgleichung

Reaktionsgleichung von HRID 229731
[CH3:1][CH:2]1[CH2:11][C:10]2[N:9]=[N:8][C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=3)=[CH:6][C:5]=2[C:4](=[O:22])[CH2:3]1.[Br-].C(=O)(O)[O-].[Na+]>C(OCC)(=O)C>[CH3:1][C:2]1[CH:3]=[C:4]([OH:22])[C:5]2[CH:6]=[C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=3)[N:8]=[N:9][C:10]=2[CH:11]=1

Komponenten

5

Edukt 3

HCID 259Bromide ionHCID 516892Sodium BicarbonateHCID 100180127-methyl-3-(3-trifluoromethylphenyl)-7,8-dihydro-6H-cinnolin-5-one

Produkt 1

HCID 135458024HCID 135458024, VerbindungAusbeute 5,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel3×

Versuchsvorschrift

To an ethyl acetate solution (1 mL) of 7-methyl-3-(3-trifluoromethylphenyl)-7,8-dihydro-6H-cinnolin-5-one (306 mg, 1.0 mmol) obtained in Example 66 was added cupuric bromide (446 mg, 2.0 mmol), followed by reaction under heating and refluxing for 8 hours, adding saturated sodium bicarbonate aqueous solution (2 mL) to the reaction liquid and extraction with ethyl acetate. To residue obtained after concentration of an organic layer under reduced pressure was added ethyl acetate (1 mL) and filtered off solid obtained to get an objective product (17 mg, 5.5%) as yellow solid.

Aufarbeitung

  1. customfollowed by reaction
  2. temperatureunder heating
  3. temperaturerefluxing for 8 hours
  4. customTo residue obtained after concentration of an organic layer under reduced pressure
  5. filtrationfiltered off solid
  6. customobtained

Quellen und Nachweise

ORD-Eintrag
ord-ff26126a4628438c9be7a02cf30b4270
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07563893B2

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