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

HRID 52223ノート

反応式

HRID 52223 の反応式
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

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 214636572-Chloro-1-(chloromethyl)-4-(trifluoromethyl)benzeneHCID 136048655HCID 136048655、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-4a6eb72fb28c4705a9f9530fd2d6c138
出典データセット
uspto-grants-1997_04
特許番号
US05616594

反応ノート

読み込み中…