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

HRID 23319

반응식

HRID 23319 반응식
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

참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 27832892,4,6-TrifluoropyridineHCID 178481859HCID 178481859, 화합물

생성물 1

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

시약·촉매·용매 3

HCID 7914Diisopropyl Ether용매HCID 31347Sulfolane용매HCID 22335286Ethyl acetate pentane용매

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fe12c4b6675946fe8455049849d267c1
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06852673B2

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