참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 3-Iodopyridine-4-carboxylic acid | HCID 619275 | — |
| 반응물 | 2-Methylphenyl boronic acid | HCID 2733267 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | 3-(2-Methylphenyl)-4-pyridinecarboxylic acid | HCID 22000066 | 75.7% |
반응 단계
To a suspension of 1.05 g (4.21 mmol) 3-iodo-isonicotinic acid in 15 ml dimethoxyethane were added successively 0.243 g tetrakis(triphenylphosphine)palladium(0), 4.2 ml 2 M sodium carbonate solution in water and 0.69 g (5.05 mmol) o-tolylboronic acid. The mixture was heated under argon at 80° C. for 18 h. After cooling to room temperature the phases were separated and the organic phase was washed twice with water (pH=9). The combined aqueous layers were than adjusted to pH=3 and extracted with five portions ethyl acetate. The combined organic layers were washed with brine, dried (magnesium sulfate) and evaporated. Chromatography of the residue afforded 0.68 g (75%) of the title compound as pale yellow crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06225316B1 |
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| 출처 데이터셋 | uspto-grants-2001_05 |
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| ORD ID | ord-235b2a2d7eb04c3789284bd5fa903a25 |
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| 출처 메모 | uspto-grants-2001_05 |
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