Methanol → 4,6-Diaminonicotinonitrile

HRID 617924

反応式

HRID 617924 の反応式
Br[C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([NH2:9])[C:3]=1[C:10]#[N:11].[H][H].C([O-])(=O)C.[K+].CO>[Pd].O1CCCC1>[NH2:8][C:6]1[CH:5]=[C:4]([NH2:9])[C:3]([C:10]#[N:11])=[CH:2][N:7]=1

参加物

7

反応物 4

HCID 887MethanolHCID 1706684,6-Diamino-2-bromo-3-pyridinecarbonitrileHCID 517044Potassium AcetateHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 2958964,6-Diaminonicotinonitrile

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A suspension of 21.3 g of 6-bromo-2,4-diamino-5-cyanopyridine (JACS, 80:2838-2840 (1958)) and 1 g of 20% palladium on charcoal in 250 mL of tetrahydrofuran was shaken in a Parr apparatus under an atmosphere hydrogen. After 2 hours, the reaction was stopped and 10 g of potassium acetate and 50 mL of methanol added. The reaction was recharged with hydrogen and shaken for 18 hours. The solvents were removed under reduced pressure and the residue crystallized from isopropyl alcohol to afford the title compound 2,4-diamino-5-cyanopyridine, mp 201-202° C.

後処理

  1. customThe solvents were removed under reduced pressure
  2. customthe residue crystallized from isopropyl alcohol

出典と根拠

ORDレコード
ord-c68c356a278b4eea9c94eb125607496a
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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