Ammonia → 2-Methyl-4-(trifluoromethoxy)benzamide

HRID 2099309ノート

反応式

HRID 2099309 の反応式
[CH3:1][C:2]1[CH:10]=[C:9]([O:11][C:12]([F:15])([F:14])[F:13])[CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].S(Cl)(Cl)=O.[NH3:20]>CN(C=O)C>[CH3:1][C:2]1[CH:10]=[C:9]([O:11][C:12]([F:15])([F:14])[F:13])[CH:8]=[CH:7][C:3]=1[C:4]([NH2:20])=[O:5]

参加物

5

反応物 3

HCID 222AmmoniaHCID 24386Thionyl ChlorideHCID 27755542-Methyl-4-(trifluoromethoxy)benzoic acid

生成物 1

HCID 27755492-Methyl-4-(trifluoromethoxy)benzamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide触媒

反応条件

温度
60 °C

実験手順

795 mg (3.61 mmol) of 2-methyl-4-(trifluoromethoxy)benzoic acid are heated under reflux with 4 ml (54.8 mmol) of thionyl chloride and one drop of DMF for 30 minutes. After cooling, the reaction solution is slowly added dropwise into an ice-cooled concentrated aqueous ammonia solution. The resulting precipitate is collected by suction filtration, taken up in 30 ml of water and stirred at 60° C. for 1 h. The mixture is allowed to cool and the solid is collected by filtration and dried in vacuo. Yield: 562 mg (71% of theory).

後処理

  1. temperatureAfter cooling
  2. filtrationThe resulting precipitate is collected by suction filtration
  3. temperatureto cool
  4. filtrationthe solid is collected by filtration
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-43dde2d096924d03a58437ed6acd3ef0
出典データセット
uspto-grants-2009_08
特許番号
US07569563B2

反応ノート

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