참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 2-Iodoselenophene | HCID 142183 | — |
| 반응물 | B-(4-Ethoxy-2,3-difluorophenyl)boronic acid | HCID 15135235 | — |
| 용매 | tert-Butyl methyl ether | HCID 15413 | — |
| 용매 | Toluene ethanol | HCID 21863594 | — |
| 생성물 | 2-(4-Ethoxy-2,3-difluorophenyl)selenophene | HCID 59456301 | — |
반응 단계
A mixture of 34.8 g (0.14 mol) of 2-iodoselenophene, 32.8 g (0.16 mol) of 4-ethoxy-2,3-difluorophenylboronic acid, 8.10 g (77.01 mmol) of tetrakis -(triphenylphosphine)palladium(0) and 300 ml of 2 N sodium carbonate soln. in 800 ml of toluene/ethanol (1:1) is heated under reflux for 23 h. The mixture is diluted with MTBE and washed with water. The aqueous phase is extracted with MTBE, and the combined organic phases are washed with 2 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:EtOAc=15:1-10:1→5:1). Further purification is carried out by recrystallisation from n-heptane; 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-0762230a08e74588a5910f25485ffb77 |
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| 출처 메모 | uspto-grants-2012_11 |
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