Hydrogen Bromide → 5-(Bromomethyl)-1H-indazole--hydrogen bromide (1/1)

HRID 1634176Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1634176
C([N:4]1[C:12]2[C:7](=[CH:8][C:9]([CH2:13]OC(=O)C)=[CH:10][CH:11]=2)[CH:6]=[N:5]1)(=O)C.[BrH:18]>>[BrH:18].[Br:18][CH2:13][C:9]1[CH:8]=[C:7]2[C:12](=[CH:11][CH:10]=1)[NH:4][N:5]=[CH:6]2

Komponenten

3

Versuchsvorschrift

A suspension of 1-acetyl-5-(acetoxymethyl)indazole (12-3) (3.0 g, 13 mmol) in aqueous hydrobromic acid (15 mL, 226 mmol) was stirred at room temperature for 25 hours. The solid was collected on a Buchner funnel and dried under vacuum for 12 hours. The filtrate was stirred at room temperature for additional 24 hours and more solid was collected. After drying under vacuum, title compound was obtained as a yellow solid (12-4, 3.48 g, 92%) which was used in the next synthesis step without further purification. 1H NMR (CDCl3) δ4.88 (s, 2H), 7.43 (d, 1H, J=8.8), 7.56 (d, 1H, J=8.8 Hz), 7.87 (s, 1H), 8.10 (s, 1H).

Aufarbeitung

  1. customThe solid was collected on a Buchner funnel
  2. customdried under vacuum for 12 hours
  3. stirringThe filtrate was stirred at room temperature for additional 24 hours
  4. custommore solid was collected
  5. customAfter drying under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-093db36fc3424b989c7b53b45a063393
Quelldatensatz
uspto-grants-2003_01
Patentnummer
US06506761B1

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