참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 2-Bromoselenophene | HCID 137013 | — |
| 반응물 | B-(4-Ethoxy-2,3-difluorophenyl)boronic acid | HCID 15135235 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Toluene ethanol | HCID 21863594 | — |
| 생성물 | 2-(4-Ethoxy-2,3-difluorophenyl)selenophene | HCID 59456301 | — |
반응 단계
A mixture of 45.0 g (0.21 mol) of 2-bromoselenophene, 52.0 g (0.26 mol) of 4-ethoxy-2,3-difluorophenylboronic acid, 20.0 g (17.3 mmol) of tetrakis(triphenylphosphine)palladium(0) and 600 ml of 2 N sodium carbonate soln. in 1100 ml of toluene/ethanol (1:1) is heated under reflux for 20 h. After cooling, the organic phase is separated off, and the aqueous phase is extracted with toluene. The combined organic phases are washed with sat. sodium hydrogencarbonate soln., 1 N hydrochloric acid and sat. sodium chloride soln. The solution is dried using sodium sulfate and concentrated to dryness. The residue is purified by column chromatography (SiO2, n-heptane:toluene=3:2). Further purification is carried out by recrystallisation from ethanol; 2-(4-ethoxy-2,3-difluorophenyl)selenophene is obtained as a beige solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08304036B2 |
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| 출처 데이터셋 | uspto-grants-2012_11 |
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| ORD ID | ord-b0d75b2282834822b4ffc49a3ff86c7a |
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| 출처 메모 | uspto-grants-2012_11 |
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