참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diisopropylamine | HCID 7912 | — |
| 반응물 | Trisodium 3,3',3''-phosphinetriyltris(benzene-1-sulphonate) | HCID 6099338 | — |
| 반응물 | 2-Methylpyrimidine-5-boronic acid | HCID 45787274 | — |
| 반응물 | 2-Chloro-6-(2,4-difluorophenyl)isonicotinic acid | HCID 82305710 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-(2,4-Difluorophenyl)-6-(2-methylpyrimidin-5-yl)isonicotinic acid | HCID 67339022 | — |
반응 단계
To a solution of 2-chloro-6-(2,4-difluorophenyl)isonicotinic acid (0.10 g, 0.37 mmol) in DMF (1.9 mL) and water (0.6 mL) were added (2-methylpyrimidin-5-yl)boronic acid (0.31 g, 2.23 mmol), palladium(II)acetate (12.5 mg, 0.06 mmol), 3,3′,3″-phosphinidynetris(benzenesulfonic acid) trisodium salt (95.0 mg, 0.17 mmol) and diisopropylamine (0.19 mL, 1.30 mmol). The mixture was heated to 80° C. After 2 h, the mixture was filtered and the filtrate was purified by reverse phase chromatography (C-18, 95% water/acetonitrile→25% water/acetonitrile with 0.1% trifluoroacetic acid). To the product fractions was added HCl (2.0 M in ether) and the mixture was concentrated to give the hydrochloride salt of the title compound. MS 328.1 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08598209B2 |
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| 출처 데이터셋 | uspto-grants-2013_12 |
|---|
| ORD ID | ord-a6351b7a675d4686931e681a64c80b55 |
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| 출처 메모 | uspto-grants-2013_12 |
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