참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trimethyl((tributylstannyl)ethynyl)silane | HCID 639663 | — |
| 반응물 | Methyl 4-(acetylamino)-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylate | HCID 67210962 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | HCID 59432138 | HCID 59432138 | 21.2% |
반응 단계
4-Acetylamino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)-pyridine-2-carboxylic acid methyl ester (0.8 g, 2.061 mmol), trimethyl((tributylstannyl)ethynyl)silane (1.596 g, 4.12 mmol), and bis(triphenylphosphine)palladium(II) dichloride (0.145 g, 0.206 mmol) were combined in 1,2-dichloroethane (2 mL) and heated in a CEM microwave reactor at 130° C. for 15 min. The cooled reaction mixture was purified by flash chromatography on silica gel (hexane/ethyl acetate gradient) to yield the title compound (0.196 g, 21.1% yield). 1H NMR (CDCl3) δ 9.03 (s, 1H), 8.4 (br s, 1H), 7.67 (m, 1H), 7.24 (m, 1H), 4.0 (s, 3H), 3.99 (d, 3H), 2.29 (s, 3H), 0.36 (s, 9H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08658791B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-10ad08901c644a4b96f848dec48b2c31 |
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| 출처 메모 | uspto-grants-2014_02 |
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