Formic Acid → 2,4-Diaminonicotinaldehyde
反応式
[NH2:1][C:2]1[CH:7]=[C:6]([NH2:8])[C:5](C#N)=[CH:4][N:3]=1.[CH:11]([OH:13])=O.[H][H]>[Ni].O>[NH2:1][C:2]1[N:3]=[CH:4][CH:5]=[C:6]([NH2:8])[C:7]=1[CH:11]=[O:13]参加物
6
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.
後処理
- customwas consumed
- customThe solvents were removed under reduced pressure
- additionthe residue treated with 17 mL of concentrate HCl
- filtrationfiltered
- washwashed with isopropyl alcohol
- customdried
- customCrystallization from ethanol
出典と根拠
- ORDレコード
- ord-28134d97e9994bbca659cba3b394ce10
- 出典データセット
- uspto-grants-1999_09
- 特許番号
- US05952342
反応ノート
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