Reaktion #2277085

Reaktionsgleichung

2,5,6-trichloronicotinamide

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title compound

Ausbeute 99.2%

2,5,6-Trichloronicotinonitrile

Ausbeute 99.2%

Lösungsmittel

POCl3

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction was then cooled to room temperature
2. 2
   Sonstigethe POCl3 was removed under vacuum
3. 3
   workup.ADDITIONice water (50 ml) was then added
4. 4
   workup.ADDITIONfollowed by the careful addition of an aqueous solution of Na2CO3 until pH 8
5. 5
   TrocknenThe organic fraction was then dried over Na2SO4
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated

Vorschrift

A suspension of 2,5,6-trichloronicotinamide (Method 45, 2.3 g, 10.2 mmol) in POCl3 (20 ml) was heated to 90° C. for 1 hour. The reaction was then cooled to room temperature, and the POCl3 was removed under vacuum. The resulting residue was taken up in DCM (50 ml) and ice water (50 ml) was then added, followed by the careful addition of an aqueous solution of Na2CO3 until pH 8 was achieved. The organic fraction was then dried over Na2SO4, filtered, and concentrated to give the title compound (2.1 g, 80%) which was used without further purification. 1H NMR (400 MHz, CD3OD) δ 8.54 (s, 1H).

Quelle