2-氰基吡啶 → 2-脒基吡啶盐酸盐

HRID 487275

反应方程式

HRID 487275 反应方程式
[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]

参与物

5

反应物 2

HCID 75222-氰基吡啶HCID 25517氯化铵

产物 1

HCID 124036152-脒基吡啶盐酸盐收率 94.2%

试剂、催化剂与溶剂 2

HCID 10942334甲醇钠催化剂HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-8c89d28882ec4d119741ec8fd10c6cd2
来源数据集
uspto-grants-1994_03
专利号
US05294612

关联笔记

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