関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | 2,3-Dichloropropene | HCID 6565 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-(Trifluoromethyl)phenylcyanamide | HCID 11074102 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(3-(trifluoromethyl)phenyl)-N-(2-chloro-2-propenyl)cyanamide | HCID 21480055 | 99.1% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05648533 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-68dee3052fa64740bd0a018fac86481b |
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| 出典メモ | uspto-grants-1997_07 |
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