참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl Acrylate | HCID 7294 | — |
| 반응물 | Tri-o-tolylphosphine | HCID 80271 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 반응물 | 6-Bromo-3-pyridinecarboxaldehyde | HCID 11769234 | — |
| 촉매 | Palladium, di-mu-chlorobis(eta3-2-propenyl)di- | HCID 61538 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Ethyl (2E)-3-(5-formyl-2-pyridinyl)-2-propenoate | HCID 86628160 | 93.7% |
반응 단계
A mixture of 2-bromo-5-formylpyridine (500 mg, 2.6 mmol), methyl acrylate (0.6 ml, 6.5 mmol), tri-(o-tolyl)phosphine (80 mg, 0.26 mmol), allyl palladium (II) chloride dimer (47 mg, 0.13 mmol) and sodium acetate (1.08 g, 8 mmol) in DMF (10 ml) was heated at 170° C. in a microwave reactor for 0.75 h. The reaction mixture was filtered through Celite® then diluted with DCM and water. The organic phase was dried, concentrated in vacuo and purified by chromatography to give the title compound as a white solid (50 mg). δH (CDCl3, 250 MHz) 10.14 (1H, s), 9.09 (1H, d), 8.19 (1H, dd), 7.72 (1H, d), 7.57 (1H, d), 7.08 (1H, d), 3.85 (3H, s). MS (ES): MH+ 192.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08536182B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
|---|
| ORD ID | ord-c0809180160c4ca9954d8ce9512a8b6f |
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| 출처 메모 | uspto-grants-2013_09 |
|---|
