반응 #705107

반응 방정식

2,4-diamino-5-cyanopyridine

formic acid

hydrogen

→

title compound

2,4-Diaminonicotinaldehyde

용매

water

반응 조건

후처리

1. 1
   기타was consumed
2. 2
   기타The solvents were removed under reduced pressure
3. 3
   workup.ADDITIONthe residue treated with 17 mL of concentrate HCl
4. 4
   여과filtered
5. 5
   세척washed with isopropyl alcohol
6. 6
   기타dried
7. 7
   기타Crystallization from ethanol

실험 절차

A suspension of 13.4 g of 2,4-diamino-5-cyanopyridine from Example 14, 2 g of Raney nickel catalyst, 40 mL of 97-100% formic acid, and 80 mL of water were shaken in a Parr apparatus under an atmosphere of nitrogen until the requisite amount of hydrogen was consumed. The solvents were removed under reduced pressure and the residue treated with 17 mL of concentrate HCl. The resulting pink solid was slurried in a small amount of water, filtered, washed with isopropyl alcohol, followed by diethylether, and dried. Crystallization from ethanol afforded 6.5 g of the title compound 2,4-diaminonicotinaldehyde.

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