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

HRID 366299

반응식

HRID 366299 반응식
C[O-].[K+].[CH3:4][N:5]1[C:9]([O:10][C:11]2[CH:16]=[C:15]([O:17][C:18]3N(C)N=C(C(F)(F)F)C=3)[CH:14]=[C:13]([O:28][C:29]3[N:33]([CH3:34])[N:32]=[C:31]([C:35]([F:38])([F:37])[F:36])[CH:30]=3)[N:12]=2)=[CH:8][C:7]([C:39]([F:42])([F:41])[F:40])=[N:6]1>CO>[CH3:34][N:33]1[C:29]([O:28][C:13]2[CH:14]=[C:15]([O:17][CH3:18])[CH:16]=[C:11]([O:10][C:9]3[N:5]([CH3:4])[N:6]=[C:7]([C:39]([F:40])([F:41])[F:42])[CH:8]=3)[N:12]=2)=[CH:30][C:31]([C:35]([F:38])([F:36])[F:37])=[N:32]1

참가 물질

4

반응물 2

HCID 158696782,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridineHCID 23664618Potassium methoxide

생성물 1

HCID 225726302,6-Bis(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxypyridine수율 43.4%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A 3 ml aliquot of a 25 % solution of potassium methylate (10 mmol) in dry methanol is added to a solution of 5.7 g (10 mmol) 2,4,6-tris-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine in 20 ml anhydrous methanol. After 2 hours at ambient temperature, the reaction mixture is heated to reflux. The solvent is removed under reduced pressure and ethyl acetate is added to the residue. The mixture is washed with a 2 N sodium hydroxide solution. After drying and filtration of the organic layer, the solvents are removed and the residue is washed with diisopropyl ether and pentane. Colorless crystals (1.9 g, 43 % yield) of melting point 107° C. are obtained.

후처리

  1. temperaturethe reaction mixture is heated to reflux
  2. customThe solvent is removed under reduced pressure and ethyl acetate
  3. additionis added to the residue
  4. washThe mixture is washed with a 2 N sodium hydroxide solution
  5. customAfter drying
  6. filtrationfiltration of the organic layer
  7. customthe solvents are removed
  8. washthe residue is washed with diisopropyl ether and pentane

출처 및 근거

ORD 기록
ord-6759362e203b434a933ffc01546fab73
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06130188

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