참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Piperidine | HCID 8082 | — |
| 반응물 | 3,4-Dichlorobenzaldehyde | HCID 22710 | — |
| 반응물 | tert-Butyl cyanoacetate | HCID 70693 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | (E)-tert-butyl 2-cyano-3-(3,4-dichlorophenyl)acrylate | HCID 68751356 | 81.7% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08877815B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-1491605790b04672bdfb6bed058d5069 |
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| 출처 메모 | uspto-grants-2014_11 |
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