참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Methyl Acrylate | HCID 7294 | — |
| 반응물 | Tri-o-tolylphosphine | HCID 80271 | — |
| 반응물 | 5-Bromo-2-(trifluoromethyl)pyrimidine | HCID 33697963 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | methyl (2E)-3-[2-(trifluoromethyl)-5-pyrimidinyl]-2-propenoate | HCID 21936364 | 98% |
반응 단계
A mixture of 5-bromo-2-(trifluoromethyl)pyrimidine (900 mg, 3.97 mmol), methyl 2-propenoate (0.533 mL, 5.95 mmol), Pd(OAc)2 (44.5 mg, 0.198 mmol), tri-o-tolylphosphine (241 mg, 0.793 mmol) and TEA (1.105 mL, 7.93 mmol) in DMF (6 mL) under argon was heated at 130° C. for 1 h. After cooling to room temperature, water (40 mL) was added to the reaction mixture and then extracted by EA (3×50 mL). The organic phase was washed with brine, dried over MgSO4 and evaporated in vacuo to afford the title compound (900 mg, 3.88 mmol, 98% yield) as a yellow solid. LCMS: rt=2.67 min, [M+H+]=233
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09174968B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-b6b915b6fcc941649beb9ad9379077c6 |
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| 출처 메모 | uspto-grants-2015_11 |
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