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

HRID 487275

반응식

HRID 487275 반응식
[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]

참가 물질

5

반응물 2

HCID 7522Pyridine-2-carbonitrileHCID 25517Ammonium Chloride

생성물 1

HCID 12403615Pyridine-2-carboximidamide hydrochloride수율 94.2%

시약·촉매·용매 2

HCID 10942334Sodium Methoxide촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8c89d28882ec4d119741ec8fd10c6cd2
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05294612

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