Formic Acid → 2,4-Diaminonicotinaldehyde

HRID 617925

反応式

HRID 617925 の反応式
[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

反応物 3

HCID 284Formic AcidHCID 2958964,6-DiaminonicotinonitrileHCID 178418361HCID 178418361、化合物

生成物 1

HCID 218500292,4-Diaminonicotinaldehyde

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 962Water溶媒

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

  1. customwas consumed
  2. customThe solvents were removed under reduced pressure
  3. additionthe residue treated with 17 mL of concentrate HCl
  4. filtrationfiltered
  5. washwashed with isopropyl alcohol
  6. customdried
  7. 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

関連ノート

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