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

HRID 1266921ノート

反応式

HRID 1266921 の反応式
[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

参加物

8

反応物 4

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

生成物 1

HCID 185447832-Fluoro-6-(4-trifluoromethylphenoxy)pyridine収率 60%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒2 回HCID 8058Hexane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fe7a0e6e858046bdbafefd5e41082ec3
出典データセット
uspto-grants-2003_04
特許番号
US06551682B1

反応ノート

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