碘 → 2-氨基-3-甲基-5-碘吡啶

HRID 226355

反应方程式

HRID 226355 反应方程式
[CH3:1][C:2]1[C:3]([NH2:8])=[N:4][CH:5]=[CH:6][CH:7]=1.S(=O)(=O)(O)O.[I:14](O)(=O)(=O)=O.II.[O-]S([O-])(=S)=O.[Na+].[Na+]>O.CC(O)=O>[I:14][C:6]1[CH:7]=[C:2]([CH3:1])[C:3]([NH2:8])=[N:4][CH:5]=1

参与物

8

反应物 5

HCID 807碘HCID 1118四氧化硫HCID 153472-氨基-3-甲基吡啶HCID 24477硫代硫酸钠HCID 65185高碘酸

产物 1

HCID 9595862-氨基-3-甲基-5-碘吡啶收率 174.9%

试剂、催化剂与溶剂 2

HCID 176醋酸溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
80 °C

实验过程

To a solution of 3-methyl-2-pyridineamine (10 g) in a mixed solution of AcOH (60 mL), water (12 mL), and sulfuric acid (4.2 mL) was added periodic acid dehydrate (4.22 g) and iodine (9.39 g), and the mixture was heated at 80° C. for 2 hours. The reaction mixture was poured into 5% Na2S2O3 aq solution and extracted with ether. The organic layer was washed with 1N NaOH aq solution and brine, and dried over Na2SO4. The solvent was removed in vacuo and obtained residual solid was recrystallized with EtOH to give 5-iodo-3-methyl-2-pyridinamine (9.00 g) as pale yellow powder.

后处理

  1. extractionextracted with ether
  2. washThe organic layer was washed with 1N NaOH aq solution and brine
  3. dry with materialdried over Na2SO4
  4. customThe solvent was removed in vacuo
  5. customobtained residual solid
  6. customwas recrystallized with EtOH

来源与证据

ORD记录
ord-53f55ca96c1d4c3cab9aef891b414de3
来源数据集
uspto-grants-2009_07
专利号
US07557127B2

关联笔记

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