Potassium Nitrate → 3-Chloro-2,4-bis(pyridin-3-yloxy)-6-nitroaniline

HRID 13256

反応式

HRID 13256 の反応式
[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]

参加物

4

反応物 2

HCID 24434Potassium NitrateHCID 231456963-Chloro-2,4-bis(pyridin-3-yloxy)aniline

生成物 1

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

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-7509b6cd74074027827b34a583c39e19
出典データセット
uspto-grants-2010_06
特許番号
US07728025B2

関連ノート

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