2-Amino-6-chloropyridine-3,5-dicarbonitrile → 2-Aminopyridine-3,5-dicarbonitrile

HRID 842705

反応式

HRID 842705 の反応式
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([C:10]#[N:11])=[C:4](Cl)[N:3]=1>[Pd].O1CCOCC1>[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([C:10]#[N:11])=[CH:4][N:3]=1

参加物

4

反応物 1

HCID 2959012-Amino-6-chloropyridine-3,5-dicarbonitrile

生成物 1

HCID 2959122-Aminopyridine-3,5-dicarbonitrile

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 2-amino-6-chloro-3,5-dicyanopyridine (Synth. Comm. 1993, 2605, 15.0 g, 84 mmol) and 10% palladium on carbon (10.0 g) in dioxane (150 mL) was shaken on a Parr apparatus under hydrogen (55 psi) for 16 h. More catalyst (7.5 g) was added and after a further 4 h the reaction mixture was filtered through celite washing through with ethanol and evaporated in vacuo. The residue was partitioned between methylene chloride and 1 M HCl. The insoluble material was collected by filtration and dried to give the title compound. The methylene chloride layer was washed with brine, dried (Na2SO4) and evaporated in vacuo to give additional product:

後処理

  1. filtrationwas filtered through celite
  2. washwashing through with ethanol
  3. customevaporated in vacuo
  4. customThe residue was partitioned between methylene chloride and 1 M HCl
  5. filtrationThe insoluble material was collected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-a57ce74854b24acfbc7930dae628fd29
出典データセット
uspto-grants-2002_04
特許番号
US06376499B1

関連ノート

読み込み中…