反応 #3512

反応方程式

2,4-diamino-5-cyanopyridine

formic acid

hydrogen

→

title compound

2,4-Diaminonicotinaldehyde

溶媒

water

反応条件

後処理

1. 1
   その他was consumed
2. 2
   その他The solvents were removed under reduced pressure
3. 3
   workup.ADDITIONthe residue treated with 17 mL of concentrate HCl
4. 4
   ろ過filtered
5. 5
   洗浄washed with isopropyl alcohol
6. 6
   その他dried
7. 7
   その他Crystallization from ethanol

実験手順

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.

出典