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

HRID 251853노트

반응식

HRID 251853 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 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-c8e79eabcc134568a8b02a07271b2636
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07867992B2

반응 노트

불러오는 중…