Ammonia → 6-Bromopyridine-2-carboxamide

HRID 1717680

Reaktionsgleichung

Reaktionsgleichung von HRID 1717680
[Br:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=O)[CH:5]=[CH:4][CH:3]=1.[NH3:11]>S(Cl)(Cl)=O.O1CCOCC1>[Br:1][C:2]1[N:7]=[C:6]([C:8]([NH2:11])=[O:10])[CH:5]=[CH:4][CH:3]=1

Komponenten

5

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

6-Bromopicolinic acid (1000 mg, 4.95 mmol) was suspended in thionyl chloride (15 mL) and heated at 70° C. for 5 h. The reaction was cooled to room temperature and the volatiles were condensed under reduced pressure. A solution of ammonia (2M in dioxane (15 mL) was added to the residue and then the solvents were removed under reduced pressure. The crude residue was purified by MPLC with a gradient of 0 to 20% MeOH/dichloromethane to give 6-Bromo-pyridine-2-carboxylic acid amide as a white powder (555 mg, 45%). MS ES (MH+=201.01203.0).

Aufarbeitung

  1. temperatureThe reaction was cooled to room temperature
  2. customcondensed under reduced pressure
  3. customthe solvents were removed under reduced pressure
  4. customThe crude residue was purified by MPLC with a gradient of 0 to 20% MeOH/dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-ef965202b9f4400aa9f46cf1ee70eb7f
Quelldatensatz
uspto-grants-2010_09
Patentnummer
US07803956B2

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