一甲胺 → 4-甲氨基-3-硝基吡啶

HRID 912

反应方程式

HRID 912 反应方程式
CO[C:3]1[CH:8]=[CH:7][N:6]=[CH:5][C:4]=1[N+:9]([O-:11])=[O:10].[CH3:12][NH2:13]>CCO>[CH3:12][NH:13][C:3]1[CH:8]=[CH:7][N:6]=[CH:5][C:4]=1[N+:9]([O-:11])=[O:10]

参与物

4

反应物 2

HCID 6329一甲胺HCID 3558324-甲氧基-3-硝基吡啶

产物 1

HCID 5560164-甲氨基-3-硝基吡啶收率 88%

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂3 次

反应条件

温度
140 °C

实验过程

4-Methoxy-3-nitropyridine (8.17 g, 53.0 mmol) was transferred to a bomb in EtOH (5-10 mL). To this was added a solution of methylamine in EtOH (26.4 mL, 8.03M, 0.212 mol). The bomb was sealed and lowered into an oil bath at 120° C. The bath temperature fell to 90° C. and remained that way for 2 hours. The temperature was raised to 140° C. over 0.5 hour and held there 0.5 hour. The contents were transferred to a flask with EtOH (not very soluble) and the solvent was evaporated. Flash chromatography on silica gel with a gradient of CH2Cl2 /CH3OH gave 7.17 g (88%) of 4-methylamino-3-nitropyridine as a yellow solid: mp 155°-158° C.

后处理

  1. customThe bomb was sealed
  2. customlowered into an oil bath at 120° C
  3. customfell to 90° C.
  4. customfor 2 hours
  5. custom(not very soluble) and the solvent was evaporated

来源与证据

ORD记录
ord-2a0bdad4b0df4772b53e846d39972e90
来源数据集
uspto-grants-1998_03
专利号
US05723468

关联笔记

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