碘 → Methyl 4-amino-3-iodo-5-nitrobenzoate

HRID 446225

反应方程式

HRID 446225 反应方程式
[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7]([NH2:10])=[C:6]([N+:11]([O-:13])=[O:12])[CH:5]=1.[I:15]I>C(O)C.[O-]S([O-])(=O)=O.[Ag+].[Ag+]>[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:5]=[C:6]([N+:11]([O-:13])=[O:12])[C:7]([NH2:10])=[C:8]([I:15])[CH:9]=1

参与物

5

反应物 2

HCID 807碘HCID 39410084-氨基-3-硝基苯甲酸甲酯

产物 1

HCID 67512142Methyl 4-amino-3-iodo-5-nitrobenzoate收率 66%

试剂、催化剂与溶剂 2

HCID 159865硫酸银催化剂HCID 702乙醇溶剂

实验过程

To a solution of 4-amino-3-nitro-benzoic acid methyl ester (4.6 g, 23.45 mmol) in ethanol (120 mL) was added iodine (8.33 g, 32.83 mmol), followed by Ag2SO4 (10.24 g 32.83 mmol). The mixture was stirred overnight at room temperature and then filtered. The filtrate was concentrated under reduced pressure and the residue was purified by column chromatography to give 4.98 g (66%) of 4-amino-3-iodo-5-nitro-benzoic acid methyl ester.

后处理

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. customthe residue was purified by column chromatography

来源与证据

ORD记录
ord-f14f5884ca5e419d99f7cbf037dcb392
来源数据集
uspto-grants-2013_07
专利号
US08476457B2

关联笔记

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