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

HRID 1940720

反応式

HRID 1940720 の反応式
CN(C)C=O.[F:6][C:7]([F:17])([F:16])[O:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:25][C:26]1[CH:31]=[CH:30][C:29]([C:32]2[N:36]([CH3:37])[N:35]=[C:34]([C:38]3[C:43]([F:44])=[CH:42][CH:41]=[CH:40][C:39]=3[Cl:45])[N:33]=2)=[CH:28][C:27]=1[Cl:46]>O>[Cl:45][C:39]1[CH:40]=[CH:41][CH:42]=[C:43]([F:44])[C:38]=1[C:34]1[N:33]=[C:32]([C:29]2[CH:30]=[CH:31][C:26]([CH2:25][O:15][C:12]3[CH:11]=[CH:10][C:9]([O:8][C:7]([F:16])([F:17])[F:6])=[CH:14][CH:13]=3)=[C:27]([Cl:46])[CH:28]=2)[N:36]([CH3:37])[N:35]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 70015p-(Trifluoromethoxy)phenolHCID 214636485-(4-bromomethyl-3-chlorophenyl) 3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole

生成物 1

HCID 214636363-(2-chloro-6-fluorophenyl)-5-[3-chloro-4-(4-trifluoromethoxyphenoxymethyl)phenyl]-1-methyl-1H-1,2,4-triazole収率 96.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 30 ml of N,N-dimethylformamide are added 4-trifluoromethoxy phenol (0.33 g) and potassium carbonate (0.25 g) and 5-(4-bromomethyl-3-chlorophenyl)-3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole (0.70 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 0.83 g of desired compound (refractive index: 1.5701).

後処理

  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

出典と根拠

ORDレコード
ord-324ddefebfcc4635a02dced2578e459f
出典データセット
uspto-grants-1997_12
特許番号
US05700824

関連ノート

読み込み中…