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

HRID 13307노트

반응식

HRID 13307 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-37e3c2824ee24e1991bba8bd626a02a6
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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