Bromine → HCID 178498803, Verbindung

HRID 245633Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 245633
[CH3:1][O:2][C:3]([C:5]1[C:6]([NH2:15])=[C:7]([Cl:14])[CH:8]=[C:9]2[C:13]=1[NH:12][N:11]=[CH:10]2)=[O:4].[Br:16]Br>C(O)(=O)C>[CH3:1][O:2][C:3]([C:5]1[C:6]([NH2:15])=[C:7]([Cl:14])[CH:8]=[C:9]2[C:13]=1[NH:12][N:11]=[C:10]2[Br:16])=[O:4]

Komponenten

4

Edukt 2

HCID 24408BromineHCID 57990143HCID 57990143, Verbindung

Produkt 1

HCID 178498803HCID 178498803, VerbindungAusbeute 11 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a solution of 9 g (29.92 mmol) of 6-amino-5-chloro-1H-indazole-7-carboxylic acid methyl ester in 68 mL of acetic acid at 80° C., is added dropwise 2 mL (38.89 mmol) of bromine. The mixture is stirred over the night at 80° C. The solvents are evaporated and water is added to the residue. The product is precipitated at pH 5 by addition of 1N aqueous NaOH, filtrated, washed with a minimum of water and dried under high vacuum. 1 g (3.28 mmol, 11%) of pure product is obtained; LC/MS:305/306 (M+H)+.

Aufarbeitung

  1. customThe solvents are evaporated
  2. additionwater is added to the residue
  3. customThe product is precipitated at pH 5 by addition of 1N aqueous NaOH
  4. filtrationfiltrated
  5. washwashed with a minimum of water
  6. customdried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-6ba92a31314a452c9d54237e92589f82
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08658801B2

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