Reaktionsgleichung
P(Cl)(Cl)(Cl)=O.[NH2:6][C:7]1[C:8]([C:14]([NH2:16])=O)=[N:9][C:10]([I:13])=[CH:11][N:12]=1.O.[CH3:18][N:19]([CH3:22])[CH:20]=O>>[C:14]([C:8]1[C:7]([N:6]=[CH:18][N:19]([CH3:22])[CH3:20])=[N:12][CH:11]=[C:10]([I:13])[N:9]=1)#[N:16]Komponenten
5
Versuchsvorschrift
13.59 ml (146 mmol) of phosphorus oxychloride is added drop by drop at 0° C. to 11 g (41.7 mmol) of a solution of 3-amino-6-iodopyrazine-2-carboxamide in 80 ml of dimethylformamide. The reaction mixture is stirred at room temperature overnight and then poured in a beaker containing ice and a little water. The pH is adjusted to 8 with 1 N soda solution; a precipitate is formed. The mixture is allowed to gradually return to room temperature and then the solid formed is filtered, rinsed with water and dried at 50° C. to yield 10.50 g of N′-(3-cyano-5-iodopyrazine-2-yl)-N,N-dimethyl formimidamide (84%) in the form of a beige solid.
Aufarbeitung
- additionpoured in a beaker
- additioncontaining ice
- customa precipitate is formed
- customto gradually return to room temperature
- customthe solid formed
- filtrationis filtered
- washrinsed with water
- customdried at 50° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-8e059d6ea9a041a5b2e2fb4d7888fcb8
- Quelldatensatz
- uspto-grants-2014_11
- Patentnummer
- US08883821B2
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