Potassium Carbonate → 2-Fluoro-6-(4-trifluoromethylphenoxy)pyridine

HRID 1266921노트

반응식

HRID 1266921 반응식
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.C(=O)([O-])[O-].[K+].[K+].[F:18][C:19]1[CH:24]=[CH:23][CH:22]=[C:21](F)[N:20]=1.S([O-])([O-])(=O)=O.[Mg+2]>CN(C=O)C.CCCCCC.O>[F:18][C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([O:9][C:6]2[CH:5]=[CH:4][C:3]([C:2]([F:10])([F:11])[F:1])=[CH:8][CH:7]=2)[N:20]=1

참가 물질

8

반응물 4

HCID 11430Potassium CarbonateHCID 24083Sulfuric acid magnesium salt (1:1)HCID 678744-(Trifluoromethyl)phenolHCID 739342,6-Difluoropyridine

생성물 1

HCID 185447832-Fluoro-6-(4-trifluoromethylphenoxy)pyridine수율 60%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매2회HCID 8058Hexane용매

실험 절차

A reaction flask was loaded with 4-trifluoromethylphenol (8.4 g), anhydrous potassium carbonate (8.6 g), and DMF (15 ml), followed by stirring at room temperature for 15 minutes. To this mixture, 2,6-difluoropyridine (6.0 g) dissolved in DMF (15 ml) was dropwise added in one hour. Thereafter, the temperature was raised up to 60° C., and the mixture was stirred for six hours. Water was added to the reaction mixture, and extraction was carried out with hexane, followed by addition of magnesium sulfate to the extracted liquid for drying. After filtration to remove magnesium sulfate, hexane was removed by an evaporator to give 2-fluoro-6-(4-trifluoromethylphenoxy)-pyridine (8.0 g).

후처리

  1. additionwas dropwise added in one hour
  2. temperatureThereafter, the temperature was raised up to 60° C.
  3. stirringthe mixture was stirred for six hours
  4. customfor drying
  5. filtrationAfter filtration
  6. customto remove magnesium sulfate, hexane
  7. customwas removed by an evaporator

출처 및 근거

ORD 기록
ord-fe7a0e6e858046bdbafefd5e41082ec3
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06551682B1

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