Isobutyryl chloride → 6-Bromo-3-(propan-2-yl)[1,2,4]triazolo[4,3-a]pyridine--hydrogen chloride (1/1)

HRID 498074Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 498074
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][NH2:9])=[N:6][CH:7]=1.[C:10]([Cl:15])(=O)[CH:11]([CH3:13])[CH3:12]>CCCCCC>[ClH:15].[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:10]([CH:11]([CH3:13])[CH3:12])=[N:9][N:8]=2)[CH:7]=1

Komponenten

4

Edukt 2

HCID 62325Isobutyryl chlorideHCID 115356995-Bromo-2-hydrazinopyridine

Produkt 1

HCID 221701776-Bromo-3-(propan-2-yl)[1,2,4]triazolo[4,3-a]pyridine--hydrogen chloride (1/1)

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8058HexaneLösungsmittel

Versuchsvorschrift

A 500 ml three-necked round-bottomed flask equipped with a mechanical stirrer and a condenser, connected on top to a nitrogen bubbler and a thermometer, was charged with 5-bromo-pyridin-2-yl-hydrazine (43.4 g, 0.231 moles) and isobutyryl chloride (218 ml, 2.08 moles). The mixture was gently refluxed for 3 hours. The heating source was then replaced with an ice-water bath and the slurry cooled to room temperature. Hexane (220 ml) was added and the slurry stirred at room temperature for 15 minutes and filtered. The cake was washed with hexane (3×70 ml) and then dried in a vacuum-oven (35° C.) for 48 hours. The title compound was obtained as an off-white powder (58.96 g, yield 92.3%).

Aufarbeitung

  1. customA 500 ml three-necked round-bottomed flask equipped with a mechanical stirrer and a condenser
  2. temperatureThe mixture was gently refluxed for 3 hours
  3. customThe heating source was then replaced with an ice-water bath
  4. filtrationfiltered
  5. washThe cake was washed with hexane (3×70 ml)
  6. customdried in a vacuum-oven (35° C.) for 48 hours

Quellen und Nachweise

ORD-Eintrag
ord-567c3671f56e4df3955f2b4807fa3bd8
Quelldatensatz
uspto-grants-2005_09
Patentnummer
US06949652B2

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