硝酸钾 → 3-Chloro-2,4-bis(pyridin-3-yloxy)-6-nitroaniline

HRID 13256

反应方程式

HRID 13256 反应方程式
[N+:1]([O-:4])([O-])=[O:2].[K+].[Cl:6][C:7]1[C:8]([O:21][C:22]2[CH:23]=[N:24][CH:25]=[CH:26][CH:27]=2)=[C:9]([CH:11]=[CH:12][C:13]=1[O:14][C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)[NH2:10]>FC(F)(F)C(O)=O>[Cl:6][C:7]1[C:8]([O:21][C:22]2[CH:23]=[N:24][CH:25]=[CH:26][CH:27]=2)=[C:9]([C:11]([N+:1]([O-:4])=[O:2])=[CH:12][C:13]=1[O:14][C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)[NH2:10]

参与物

4

反应物 2

HCID 24434硝酸钾HCID 231456963-Chloro-2,4-bis(pyridin-3-yloxy)aniline

产物 1

HCID 231457143-Chloro-2,4-bis(pyridin-3-yloxy)-6-nitroaniline

试剂、催化剂与溶剂 1

HCID 6422三氟乙酸溶剂

实验过程

315 mg of potassium nitrate was added to a trifluoroacetic acid (20 ml) solution of 891 mg of 3-chloro-2,4-bis(pyridin-3-yloxy)aniline, and the reaction liquid was stirred overnight at room temperature, and then the solvent was evaporated away under reduced pressure. The residue was diluted with ethyl acetate, washed with aqueous saturated sodium bicarbonate and saturated saline in order, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified with silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate) to obtain the entitled compound as an orange solid.

后处理

  1. customthe reaction liquid
  2. customthe solvent was evaporated away under reduced pressure
  3. additionThe residue was diluted with ethyl acetate
  4. washwashed with aqueous saturated sodium bicarbonate and saturated saline in order
  5. dry with materialdried with anhydrous magnesium sulfate
  6. customThe solvent was evaporated away under reduced pressure
  7. customthe resulting residue was purified with silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate)

来源与证据

ORD记录
ord-7509b6cd74074027827b34a583c39e19
来源数据集
uspto-grants-2010_06
专利号
US07728025B2

关联笔记

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