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Water → 2,6-Difluoro-nicotinic acid methyl ester

HRID 1024183
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HRID 1024183 반응식
[F:1][C:2]1[N:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.O.[C:18](=O)([O-])[O-].[K+].[K+]>CO>[CH3:18][O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][C:9]([F:11])=[N:10][C:2]=1[F:1]
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참가 물질

6

반응물 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 11430Potassium CarbonateHCID 105830702,6-Difluoropyridine-3-carboxylic acid

생성물 1

HCID 108449402,6-Difluoro-nicotinic acid methyl ester

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To 2,6-difluoro-nicotinic acid (59, 5.60 g, 0.0352 mol) in methanol (60.0 mL) was added concentrated sulfuric acid (1.0 mL, 0.019 mol). The reaction was heated to reflux overnight, then poured into water, basified with 1M potassium carbonate to pH around 9, and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated to give a yellow oil (60, 3.5 g, 57.0%).

후처리

  1. temperatureThe reaction was heated
  2. temperatureto reflux overnight
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customto give a yellow oil (60, 3.5 g, 57.0%)

출처 및 근거

ORD 기록
ord-457d5bb45a014f8c8eb941300a3b354c
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722702B2

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