Potassium Nitrate → 5-Fluoro-4-(6-ethanesulfonyl-pyridin-3-yloxy)-2-nitro-phenylamine

HRID 13307ノート

反応式

HRID 13307 の反応式
[N+:1]([O-:4])([O-])=[O:2].[K+].[F:6][C:7]1[CH:8]=[C:9]([NH2:25])[CH:10]=[CH:11][C:12]=1[O:13][C:14]1[CH:15]=[N:16][C:17]([S:20]([CH2:23][CH3:24])(=[O:22])=[O:21])=[CH:18][CH:19]=1>FC(F)(F)C(O)=O>[F:6][C:7]1[C:12]([O:13][C:14]2[CH:15]=[N:16][C:17]([S:20]([CH2:23][CH3:24])(=[O:22])=[O:21])=[CH:18][CH:19]=2)=[CH:11][C:10]([N+:1]([O-:4])=[O:2])=[C:9]([NH2:25])[CH:8]=1

参加物

4

反応物 2

HCID 24434Potassium NitrateHCID 231456053-Fluoro-4-(6-ethanesulfonyl-pyridin-3-yloxy)-phenylamine

生成物 1

HCID 231450955-Fluoro-4-(6-ethanesulfonyl-pyridin-3-yloxy)-2-nitro-phenylamine

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

3.8 g of potassium nitrate was added to a trifluoroacetic acid (100 ml) solution of 10.5 g of 3-fluoro-4-(6-ethanesulfonyl-pyridin-3-yloxy)-phenylamine, and the reaction liquid was stirred for 1 hour at room temperature, and 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 sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/2) to obtain the entitled compound.

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 sodium sulfate
  6. customThe solvent was evaporated away under reduced pressure
  7. customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/2)
  8. customto obtain the entitled compound

出典と根拠

ORDレコード
ord-37e3c2824ee24e1991bba8bd626a02a6
出典データセット
uspto-grants-2010_06
特許番号
US07728025B2

反応ノート

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