참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ethyl 2-bromobenzoate | HCID 80186 | — |
| 반응물 | Benzenemethanamine, ar-ethenyl-N,N-dimethyl- | HCID 519956 | — |
| 촉매 | Tri-o-tolylphosphine | HCID 80271 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Ethyl 2-(E-2-(4-(N,N-dimethylaminomethyl)phenyl)ethen-1-yl)benzoate | HCID 11120439 | 63.5% |
반응 단계
18.8 g (82 mmol) of ethyl 2-bromobenzoate, 17.2 g (107 mmol) of 4-(N,N,-dimethylaminomethyl)styrene [sic], 20.7 g (205 mmol) of triethylamine, 0.36 g of palladium(II) acetate and 0.96 g of tri(o-tolyl)phosphine were mixed in 200 ml of dimethylformamide and, after addition of 1 ml of water, stirred at 140° C. for 3 h. The reaction mixture was then concentrated in vacuo, and the resulting residue was partitioned between ethyl acetate and water. The organic phase was separated off, washed with water, dried and concentrated in vacuo. The residue was then recrystallized from petroleum ether. 16.1 g (63%) of the product were obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06753327B1 |
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| 출처 데이터셋 | uspto-grants-2004_06 |
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| ORD ID | ord-e2ba3e3780ca467db588c06050d34043 |
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| 출처 메모 | uspto-grants-2004_06 |
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