Pyridine-2-carbonitrile → Pyridine-2-carboximidamide hydrochloride

HRID 487275

反応式

HRID 487275 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)#[N:2].[Cl-:9].[NH4+:10]>CO.C[O-].[Na+]>[ClH:9].[N:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[C:1]([NH2:10])=[NH:2]

参加物

5

反応物 2

HCID 7522Pyridine-2-carbonitrileHCID 25517Ammonium Chloride

生成物 1

HCID 12403615Pyridine-2-carboximidamide hydrochloride収率 94.2%

試薬・触媒・溶媒 2

HCID 10942334Sodium Methoxide触媒HCID 887Methanol溶媒

実験手順

To a solution of 2-cyanopyridine (20.0 g, 0.19 mol) in methanol (300 ml) under argon was added sodium methoxide (0.5 g). The reaction mixture was stirred at room temperature for 24 hours, then ammonium chloride (10.7 g, 0.2 mol) was added. The mixture was stirred at room temperature for 3.5 hours and the solvent was removed in vacuo. The residue was diluted with isopropanol (20 ml) and ether (400 ml) and a solid was collected by filtration to afford 28.2 g (87%) of 2-pyridinecarboxamidine hydrochloride as a white solid, m.p. 141°-142° C. when dried at 40° C. in high vacuum.

後処理

  1. stirringThe mixture was stirred at room temperature for 3.5 hours
  2. customthe solvent was removed in vacuo
  3. additionThe residue was diluted with isopropanol (20 ml) and ether (400 ml)
  4. filtrationa solid was collected by filtration

出典と根拠

ORDレコード
ord-8c89d28882ec4d119741ec8fd10c6cd2
出典データセット
uspto-grants-1994_03
特許番号
US05294612

関連ノート

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