Potassium Carbonate → 2,3-Difluoro-1-(6-methanesulfonyl-pyridin-3-yloxy)-4-nitro-benzene

HRID 13332

반응식

HRID 13332 반응식
[CH3:1][S:2]([C:5]1[N:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=1)(=[O:4])=[O:3].C(=O)([O-])[O-].[K+].[K+].CN1CCCC1=O.[F:25][C:26]1[C:31]([F:32])=[C:30](F)[CH:29]=[CH:28][C:27]=1[N+:34]([O-:36])=[O:35]>C(OCC)(=O)C>[F:32][C:31]1[C:26]([F:25])=[C:27]([N+:34]([O-:36])=[O:35])[CH:28]=[CH:29][C:30]=1[O:11][C:8]1[CH:9]=[N:10][C:5]([S:2]([CH3:1])(=[O:4])=[O:3])=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 13387N-methyl-2-pyrrolidoneHCID 698711,2,3-Trifluoro-4-nitrobenzeneHCID 231451966-(Methylsulfonyl)pyridin-3-ol

생성물 1

HCID 231457962,3-Difluoro-1-(6-methanesulfonyl-pyridin-3-yloxy)-4-nitro-benzene

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
50 °C

실험 절차

112 mg of 6-methanesulfonyl-pyridin-3-ol and 100 mg of potassium carbonate were added to an N-methylpyrrolidinone (3 ml) solution of 135 mg of 2,3,4-trifluoro-nitrobenzene, and the reaction liquid was stirred at 50° C. for 1 hour. The reaction liquid was diluted with ethyl acetate, washed with water 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=1/1) to obtain the entitled compound.

후처리

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. washwashed with water and saturated saline in order
  4. dry with materialdried with anhydrous sodium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1)
  7. customto obtain the entitled compound

출처 및 근거

ORD 기록
ord-f1e825910c5e4810ac501736dcd3ce56
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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