Dimethylformamide → 3-(2-chloro-6-fluorophenyl)-5-[3-chloro-4-(4-trifluoromethylphenoxymethyl)phenyl]-1-methyl-1H-1,2,4-triazole

HRID 1940719노트

반응식

HRID 1940719 반응식
CN(C)C=O.[F:6][C:7]([F:16])([F:15])[C:8]1[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:24][C:25]1[CH:30]=[CH:29][C:28]([C:31]2[N:35]([CH3:36])[N:34]=[C:33]([C:37]3[C:42]([F:43])=[CH:41][CH:40]=[CH:39][C:38]=3[Cl:44])[N:32]=2)=[CH:27][C:26]=1[Cl:45]>O>[Cl:44][C:38]1[CH:39]=[CH:40][CH:41]=[C:42]([F:43])[C:37]=1[C:33]1[N:32]=[C:31]([C:28]2[CH:29]=[CH:30][C:25]([CH2:24][O:14][C:11]3[CH:10]=[CH:9][C:8]([C:7]([F:15])([F:16])[F:6])=[CH:13][CH:12]=3)=[C:26]([Cl:45])[CH:27]=2)[N:35]([CH3:36])[N:34]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 678744-(Trifluoromethyl)phenolHCID 214636485-(4-bromomethyl-3-chlorophenyl) 3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole

생성물 1

HCID 214635883-(2-chloro-6-fluorophenyl)-5-[3-chloro-4-(4-trifluoromethylphenoxymethyl)phenyl]-1-methyl-1H-1,2,4-triazole수율 78.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 30 ml of N,N-dimethylformamide are added 4-trifluoromethyl phenol (0.77 g) and potassium carbonate (0.72 g) and 5-(4-bromomethyl-3-chlorophenyl)-3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole (1.60 g) is added thereto at room temperature with stirring, which is stirred at 120° C. for 1 hour. On completion of the reaction, the reaction solution is cooled to room temperature, poured into water and extracted with toluene. The organic layer is washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography to give 1.50 g of desired compound (refractive index: 1.5961).

후처리

  1. additionis added
  2. stirringwhich is stirred at 120° C. for 1 hour
  3. customOn completion of the reaction
  4. temperaturethe reaction solution is cooled to room temperature
  5. extractionextracted with toluene
  6. washThe organic layer is washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe concentrate is purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-5fe1170c6854469984f2226910a6de34
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05700824

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