Potassium Carbonate → 2,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine

HRID 2229110

反応式

HRID 2229110 の反応式
F[C:2]1[CH:7]=[C:6](F)[CH:5]=[C:4](F)[N:3]=1.[OH:10][C:11]1[N:15]([CH3:16])[N:14]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:12]=1.[C:21](=[O:24])([O-])[O-].[K+].[K+]>S1(CCCC1)(=O)=O.CCCCC.C(OCC)(=O)C.C(OC(C)C)(C)C>[CH3:16][N:15]1[C:11]([O:10][C:2]2[CH:7]=[C:6]([O:10][C:11]3[N:15]([CH3:16])[N:14]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:12]=3)[CH:5]=[C:4]([O:24][C:21]3[N:15]([CH3:11])[N:14]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:12]=3)[N:3]=2)=[CH:12][C:13]([C:17]([F:20])([F:19])[F:18])=[N:14]1

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 27832892,4,6-TrifluoropyridineHCID 178481859HCID 178481859、化合物

生成物 1

HCID 158696782,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine収率 93%

試薬・触媒・溶媒 3

HCID 7914Diisopropyl Ether溶媒HCID 31347Sulfolane溶媒HCID 22335286Ethyl acetate pentane溶媒

反応条件

温度
80 °C

実験手順

A mixture of 4.8 g (36 mmol) 2,4,6-trifluoropyridine, 19.8 g (119 mmol) 5-hydroxy-1-methyl-3-trifluoromethylpyrazole and 18.1 g (131 mmol) potassium carbonate in 25 ml anhydrous sulfolane is stirred and heated to 80° C. over a period of 3 days. After cooling, the mixture is diluted with pentane/ethyl acetate (by volume ration 1/1) and filtered through a bed of silica gel. The filtrate is washed 10 times with water and the organic layer is dried over magnesium sulfate. After removal of the solvents, the residue is washed with isopropyl ether and 19.1 g (93% yield) colorless crystals of melting point 130° C. are obtained.

後処理

  1. temperatureAfter cooling
  2. filtrationfiltered through a bed of silica gel
  3. washThe filtrate is washed 10 times with water
  4. dry with materialthe organic layer is dried over magnesium sulfate
  5. customAfter removal of the solvents

出典と根拠

ORDレコード
ord-b9a85229f0c4469ba322cc2afebe7916
出典データセット
uspto-grants-2002_07
特許番号
US06420315B1

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