Potassium Iodide → N-(3-(trifluoromethyl)phenyl)-N-(2-chloro-2-propenyl)cyanamide

HRID 265733

반응식

HRID 265733 반응식
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:4]=[C:5]([NH:9][C:10]#[N:11])[CH:6]=[CH:7][CH:8]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[Cl:22][C:23]([CH2:25]Cl)=[CH2:24]>CN(C)C=O>[F:1][C:2]([F:12])([F:13])[C:3]1[CH:4]=[C:5]([N:9]([CH2:25][C:23]([Cl:22])=[CH2:24])[C:10]#[N:11])[CH:6]=[CH:7][CH:8]=1

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 65652,3-DichloropropeneHCID 11430Potassium CarbonateHCID 110741023-(Trifluoromethyl)phenylcyanamide

생성물 1

HCID 21480055N-(3-(trifluoromethyl)phenyl)-N-(2-chloro-2-propenyl)cyanamide수율 99.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

N-(3-(trifluoromethyl)phenyl)cyanamide (18.6 g) was dissolved in N,N-dimethylformamide (DMF) (93.0 g), to which powdered potassium carbonate (20.7 g) and potassium iodide (1.7 g) were added at room temperature with stirring. Further, 2,3-dichloro-1-propene (13.3 g) was added dropwise at room temperature with stirring. The mixture was heated to 50° C. and stirred at the same temperature for 1 hour. After cooling to room temperature, waster was added to the reaction mixture, which was then extracted with ethyl acetate. The organic layer was washed with water. The solvent was removed by distillation under reduced pressure, which afforded 25.8 g of N-(3-(trifluoromethyl)phenyl)-N-(2-chloro-2-propenyl)cyanamide as an oil (99% yield in appearance). The percentage areas of gas chromatography and liquid chromatography were 98% and 99%, respectively.

후처리

  1. additionwere added at room temperature
  2. stirringwith stirring
  3. stirringstirred at the same temperature for 1 hour
  4. temperatureAfter cooling to room temperature
  5. additionwaster was added to the reaction mixture, which
  6. extractionwas then extracted with ethyl acetate
  7. washThe organic layer was washed with water
  8. customThe solvent was removed by distillation under reduced pressure, which

출처 및 근거

ORD 기록
ord-68dee3052fa64740bd0a018fac86481b
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05648533

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