Bromine → HCID 178478419, Verbindung

HRID 268869

Reaktionsgleichung

Reaktionsgleichung von HRID 268869
[Cl:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[NH:4][N:3]=1.[Br:11]Br>CC(O)=O.CCOC(C)=O>[Br:11][C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][CH:7]=1)[NH:4][N:3]=[C:2]2[Cl:1]

Komponenten

5

Edukt 2

HCID 24408BromineHCID 958943-Chloro-1H-indazole

Produkt 1

HCID 178478419HCID 178478419, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a room temperature solution of 3-chloro-1H-indazole (10.0 g, 65.5 mmol) in AcOH (250 ml) was added Br2 (3.54 ml, 68.8 mmol) dropwise. The reaction mixture was stirred at room temperature for 18 hours, then diluted with EtOAc (500 ml), washed with aqueous NaOH solution (10%), saturated aqueous NaHCO3 and brine. The organic layer was dried over MgSO4, filtered, concentrated, and the residue was recrystallized from toluene. The solid was washed with hexanes and dried in vacuo affording 5-Bromo-3-chloro-1H-indazole CCXIV as a white solid (54% yield).

Aufarbeitung

  1. washwashed with aqueous NaOH solution (10%), saturated aqueous NaHCO3 and brine
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customthe residue was recrystallized from toluene
  6. washThe solid was washed with hexanes
  7. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-7e4ebfc6579e44509b9a6fc46fe0eaf7
Quelldatensatz
uspto-grants-2008_11
Patentnummer
US07446118B2

Verknüpfte Notizen

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