関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 3,4-Dichlorobenzaldehyde | HCID 22710 | — |
| 反応物 | tert-Butyl cyanoacetate | HCID 70693 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (E)-tert-butyl 2-cyano-3-(3,4-dichlorophenyl)acrylate | HCID 68751356 | 81.7% |
反応手順
A solution of tert-butyl cyanoacetate (2.52 ml, 17.63 mmol), 3,4-dichlorobenzaldehyde (2.57 g, 14.69 mmol) and piperidine (0.145 ml, 1.469 mmol) in EtOH (50 ml) was allowed to stir at 80° C. for 15 hours, and then cooled to ambient temperature. A half volume of the solvent was evaporated, and 400 ml of water was added to the resulting mixture. The precipitated solid was collected and washed with 5% iPrOH/H2O (200 ml). The solid was dried under reduced pressure to give (E)-tert-butyl 2-cyano-3-(3,4-dichlorophenyl)acrylate (3.577 g); Retention time=1.61 minutes (condition A); MS (ES+)=315.1 (m+18).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08877815B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-1491605790b04672bdfb6bed058d5069 |
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| 出典メモ | uspto-grants-2014_11 |
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