関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl 2-bromobenzoate | HCID 80186 | — |
| 反応物 | Benzenemethanamine, ar-ethenyl-N,N-dimethyl- | HCID 519956 | — |
| 触媒 | Tri-o-tolylphosphine | HCID 80271 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 2-(E-2-(4-(N,N-dimethylaminomethyl)phenyl)ethen-1-yl)benzoate | HCID 11120439 | 63.5% |
反応手順
18.8 g (82 mmol) of ethyl 2-bromobenzoate, 17.2 g (107 mmol) of 4-(N,N,-dimethylaminomethyl)styrene [sic], 20.7 g (205 mmol) of triethylamine, 0.36 g of palladium(II) acetate and 0.96 g of tri(o-tolyl)phosphine were mixed in 200 ml of dimethylformamide and, after addition of 1 ml of water, stirred at 140° C. for 3 h. The reaction mixture was then concentrated in vacuo, and the resulting residue was partitioned between ethyl acetate and water. The organic phase was separated off, washed with water, dried and concentrated in vacuo. The residue was then recrystallized from petroleum ether. 16.1 g (63%) of the product were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06753327B1 |
|---|
| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-e2ba3e3780ca467db588c06050d34043 |
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| 出典メモ | uspto-grants-2004_06 |
|---|
