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

HRID 251853ノート

反応式

HRID 251853 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溶媒

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 with 4 ml (54.8 mmol) of thionyl chloride and a drop of DMF for 30 min under reflux. After cooling the reaction mixture is added slowly 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 for 1 h at 60° C. The reaction mixture is left to cool, the solid is collected by filtration and dried under vacuum. Yield: 562 mg (71% of theory)

後処理

  1. temperatureAfter cooling the reaction mixture
  2. filtrationThe resulting precipitate is collected by suction filtration
  3. waitThe reaction mixture is left
  4. temperatureto cool
  5. filtrationthe solid is collected by filtration
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-c8e79eabcc134568a8b02a07271b2636
出典データセット
uspto-grants-2011_01
特許番号
US07867992B2

反応ノート

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