참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acrylate | HCID 8821 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 4-Bromo-3-(trifluoromethyl)phenol | HCID 22277307 | — |
| 촉매 | Palladium Chloride | HCID 24290 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Ethyl (2E)-3-[4-hydroxy-2-(trifluoromethyl)phenyl]prop-2-enoate | HCID 90442064 | — |
반응 단계
Into a 500-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed 4-bromo-3-(trifluoromethyl)phenol (5 g, 20.75 mmol, 1.00 equiv), N,N-dimethylformamide (60 mL), ethyl prop-2-enoate (10.5 g, 104.88 mmol, 5.06 equiv), PdCl2 (370 mg, 2.09 mmol, 0.10 equiv), P(tolyl)3 (1.28 g, 4.21 mmol, 0.20 equiv), DIEA (16.25 g). The resulting solution was stirred for overnight at 90° C. The resulting mixture was concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1/8). This resulted in 2.6 g (42%) of ethyl (2E)-3-[4-hydroxy-2-(trifluoromethyl)phenyl]prop-2-enoate as a light yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09067898B1 |
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| 출처 데이터셋 | uspto-grants-2015_06 |
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| ORD ID | ord-40226ac7e7a3447c9b9553d7579d2e6e |
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| 출처 메모 | uspto-grants-2015_06 |
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