참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Styrene | HCID 7501 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 2-Bromo-4-chloroanisole | HCID 521935 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 5-Chloro-2-methoxy-beta-phenylstyrene | HCID 68578765 | 35.6% |
반응 단계
Palladium acetate (21 mg, 7 mol %) was added to a solution of 2-bromo-4-chloroanisole (300 mg, 1.4 mmol), styrene (211 mg, 2 mmol), triethylamine (13 μL, 0.1 mmol) and triphenylphosphine (50 mg, 1.9 mmol) in acetonitrile (6 mL), and the mixture was refluxed for 8 hours under argon atmosphere. After the reaction mixture was cooled to room temperature, the solvent was concentrated under reduced pressure and the obtained residue was diluted with ethyl acetate (15 mL). After the solution was washed successively with 2N hydrochloric acid, water and brine, dried over anhydrous sodium sulfate, the residue obtained by evaporation of the solvent under reduced pressure was purified by column chromatography on silica gel (n-hexane:ethyl acetate=10:1) to give the title compound (118 mg, 35.6%) as a white powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07700655B2 |
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| 출처 데이터셋 | uspto-grants-2010_04 |
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| ORD ID | ord-bc323d90db4149c59ce4603da76843ae |
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| 출처 메모 | uspto-grants-2010_04 |
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