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

HRID 1011214노트

반응식

HRID 1011214 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 27755492-Methyl-4-(trifluoromethoxy)benzamide

시약·촉매·용매 1

HCID 6228Dimethylformamide촉매

반응 조건

온도
60 °C

실험 절차

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 introduced 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 at 60° C. for 1 h. The mixture is allowed to cool and the solid is collected by filtration and dried under vacuum. Yield 562 mg (71% of theory).

후처리

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

출처 및 근거

ORD 기록
ord-bcb59cb9a5c145b7a058930215a7ef10
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07977349B2

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