化工社化工社 化学情報印刷レポート · 研究参考用
Acrylonitrile → 3,5-Bis(trifluoromethyl)cinnamonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acrylonitrile | HCID 7855 | — |
| 反応物 | Di-tert-butylphenylphosphine | HCID 316378 | — |
| 反応物 | 3,5-Bis(trifluoromethyl)chlorobenzene | HCID 2769405 | — |
| 反応物 | alpha-Cyclohexylcyclohexanemethanamine | HCID 10774245 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 3,5-Bis(trifluoromethyl)cinnamonitrile | HCID 2736176 | 69% |
反応手順
0.382 g (7.2 mmol) of acrylonitrile, 38.7 mg (120 μmol) of NBu4Br, 6.7 mg (30 μmol) of palladium acetate and 26.7 mg (120 μmol) of phenyldi(t-butyl)phosphine are weighed into a Schlenk vessel. 1.49 g (6 mmol) of 3,5-bis(trifluoromethyl)chlorobenzene and 1.53 ml (7.2 mmol) of dicyclohexylmethylamine and also 3.5 ml of dimethylacetamide are then added. The Schlenk vessel is placed in a heating bath at 130° C. and the contents are stirred. After 4 hours, the contents are poured into 30 ml of water and the product is extracted by shaking with t-butyl methyl ether. After drying the organic phase over MgSO4, the solvent is removed under reduced pressure and the product is isolated. Orange oil, yield: 69%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07102046B2 |
| 出典データセット | uspto-grants-2006_09 |
| ORD ID | ord-fb848583d510498d9da13547449a7f6e |
| 出典メモ | uspto-grants-2006_09 |