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

HRID 265733

反応式

HRID 265733 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-68dee3052fa64740bd0a018fac86481b
出典データセット
uspto-grants-1997_07
特許番号
US05648533

関連ノート

読み込み中…