関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl cyanoacetate | HCID 7764 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 4-Chloro-3-Fluorobenzaldehyde | HCID 2724985 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Ethyl 3-(4-chloro-3-fluorophenyl)-2-cyanoacrylate | HCID 67338173 | 88% |
反応手順
4-Chloro-3-fluorobenzaldehyde (1.0 g, 6.3 mmol) was added to a solution of ethyl 2-cyanoacetate (0.71 g, 6.3 mmol) and piperidine (0.081 ml, 0.82 mmol) in toluene (10 mL) at room temperature. The mixture was heated at 100° C. for 7 hours. Upon cooling to room temperature, the mixture was concentrated in vacuo and rinsed with hexane to give ethyl 3-(4-chloro-3-fluorophenyl)-2-cyanoacrylate (1.4 g, 88%). LCMS (APCI+) [M+H]+253.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08846681B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-ec39c84d5e1f4e72b64dbc6f9ace4b66 |
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| 出典メモ | uspto-grants-2014_09 |
|---|
