참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2,6-Dichloro-3-iodopyridine | HCID 2736002 | — |
| 반응물 | 1-Ethoxyethene-2-boronic acid pinacol ester | HCID 21973908 | — |
| 촉매 | HCID 178454861 | HCID 178454861 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | (E)-2,6-dichloro-3-(2-ethoxyvinyl)pyridine | HCID 90332512 | 86% |
반응 단계
To a degassed solution of 2,6-dichloro-3-iodopyridine (3.0 g, 11 mmol) and (E)-2-(2-ethoxyvinyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (2.2 g, 11 mmol) in 1,4-dioxane (20 mL) and water (1.0 mL) was added CS2CO3 (7.1 g, 22 mmol) and 1,1′-bis(di-tert-butylphosphino)ferrocene palladium chloride (357 mg, 0.54 mmol) under N2 protection. The resulting mixture was heated to 70° C. and stirred at this temperature overnight. The reaction was cooled, filtered through a pad of the celite and washed with ethyl acetate. The combined filtrate was evaporated in vacuo. The resulting residue was purified using column chromatography (eluted with 0-20% EtOAc/DCM) to provide (E)-2,6-dichloro-3-(2-ethoxyvinyl)pyridine (1.96 mg, yield: 86%). MS (M+H)+: 218.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09243002B2 |
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| 출처 데이터셋 | uspto-grants-2016_01 |
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| ORD ID | ord-f0084eab7f1f4f4582ed8aabfa1a8ce1 |
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| 출처 메모 | uspto-grants-2016_01 |
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