Water → N-[4-(trifluoromethyl)phenyl]-2-(2-methoxyphenyl)acetamide

HRID 1816569

反応式

HRID 1816569 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][C:10]([OH:12])=O.C(Cl)(=O)C(Cl)=O.[F:19][C:20]([F:29])([F:28])[C:21]1[CH:27]=[CH:26][C:24]([NH2:25])=[CH:23][CH:22]=1.O>ClCCl>[F:19][C:20]([F:28])([F:29])[C:21]1[CH:22]=[CH:23][C:24]([NH:25][C:10](=[O:12])[CH2:9][C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=2[O:2][CH3:1])=[CH:26][CH:27]=1

参加物

6

反応物 4

HCID 962WaterHCID 71342-Methoxyphenylacetic acidHCID 99644-(Trifluoromethyl)anilineHCID 65578Oxalyl chloride2 回

生成物 1

HCID 2684094N-[4-(trifluoromethyl)phenyl]-2-(2-methoxyphenyl)acetamide収率 86%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

5.0 g of 2-methoxyphenylacetic acid was dissolved in 20 ml dichloromethane, and 4.6 g of oxalyl dichloride was added, and the mixture was stirred at room temperature for 3 hours. The solvent and an excessive oxalyl dichloride were evapoarated, and the residue was dissolved in 20 ml dichloromethane. Under ice-cooling, 14 g of 4-trifluoromethyl aniline was added thereto, followed by stirring at room temperature for 12 hours. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate, washed with 1N hydrochloric acid and brine, dried over anhydrous magnesium sulfate and then the solvent was evpoarated. The resulting solid was collected by filtration and washed with diethyl ether, to give 8.0 g of N-[4-(trifluoromethyl)phenyl]-2-(2-methoxyphenyl)acetamide as a colorless solid.

後処理

  1. temperatureUnder ice-cooling
  2. stirringby stirring at room temperature for 12 hours
  3. extractionthe mixture was extracted with ethyl acetate
  4. washwashed with 1N hydrochloric acid and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationThe resulting solid was collected by filtration
  7. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-1199172b4ef846d490aa9c7a8529414d
出典データセット
uspto-grants-2005_04
特許番号
US06884821B1

関連ノート

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