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

HRID 52223노트

반응식

HRID 52223 반응식
CN(C)C=O.[Cl:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([F:13])[C:8]=1[C:14]1[N:18]=[C:17]([C:19]2[CH:24]=[CH:23][C:22]([OH:25])=[C:21]([Cl:26])[CH:20]=2)[N:16]([CH3:27])[N:15]=1.C(=O)([O-])[O-].[K+].[K+].[Cl:34][C:35]1[CH:42]=[C:41]([C:43]([F:46])([F:45])[F:44])[CH:40]=[CH:39][C:36]=1[CH2:37]Cl>O>[Cl:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([F:13])[C:8]=1[C:14]1[N:18]=[C:17]([C:19]2[CH:24]=[CH:23][C:22]([O:25][CH2:37][C:36]3[CH:39]=[CH:40][C:41]([C:43]([F:44])([F:46])[F:45])=[CH:42][C:35]=3[Cl:34])=[C:21]([Cl:26])[CH:20]=2)[N:16]([CH3:27])[N:15]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 214636572-Chloro-1-(chloromethyl)-4-(trifluoromethyl)benzeneHCID 136048655HCID 136048655, 화합물

생성물 1

HCID 214636763-(2-chloro-6-fluorophenyl)-5-[3-chloro-4-(2-chloro-4-trifluoromethylbenzyloxy)phenyl]-1-methyl-1H-1,2,4-triazole수율 72.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 20 ml of N,N-dimethylformamide are added 3-(2-chloro-6-fluorophenyl)-5(3-chloro-4-hydroxyphenyl)-1-methyl-1H-1,2,4-triazole (0.70 g) and potassium carbonate (0.31 g) and 2-chloro-4-trifluoromethylbenzyl chloride (0.50 g) is added thereto at room temperature with stirring, which is stirred at 120° C. for 5 hours. On completion of the reaction, the reaction solution is cooled to room temperature, poured into water and extracted with ethyl acetate. 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 0.80 g of desired compound (melting point: 156.0°-159.0° C.).

후처리

  1. additionis added
  2. stirringwhich is stirred at 120° C. for 5 hours
  3. customOn completion of the reaction
  4. temperaturethe reaction solution is cooled to room temperature
  5. extractionextracted with ethyl acetate
  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-4a6eb72fb28c4705a9f9530fd2d6c138
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616594

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