참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | Sodium 3-cyano-6-oxo-1-phenyl-1,6-dihydropyridine-2-thiolate | HCID 11615758 | — |
| 생성물 | HCID 68808274 | HCID 68808274 | — |
반응 단계
A mixture of Example 1 (0.5 g) and Intermediate 2 (0.35 g) in MeCN (10 mL) was heated at reflux for 1.5 h. H2O (2.5 mL) was added and the resulting mixture was concentrated in vacuo. The resulting solid precipitate was recovered by filtration and dried under vacuum to give 6-oxo-2-[2-oxo-2-(pyrrolidin-1-yl)ethylsulfanyl]-1-phenyl-1,6-dihydropyridine-3-carbonitrile (0.56 g). δH (DMSO-d6) 7.998 (1H, d, J 9.5 Hz), 7.75 (3H, m), 7.55 (2H, m), 6.85 (1H, d, J 9.5 Hz), 3.86 (2H, s), 3.62-3.37 (4H, m), 2.15-1.90 (4H, m). A mixture of this material (0.38 g) and K2CO3 (0.31 g) in EtOH (7.5 mL) was heated at reflux for 2.5 h. H2O (10 mL) was added and the mixture was concentrated under vacuum. The resulting solid product was filtered, washed with water and dried in vacuo to give the title compound as an off-white solid (0.37 g). δH (DMSO-d6) 8.12 (1H, d, J 9.4 Hz), 7.66-7.50 (3H, m), 7.44 (2H, m), 7.25 (2H, br s), 6.50 (1H, d, J 9.4 Hz), 3.36 (4H, m), 1.75 (4H, m). LCMS (ES+) RT 2.84 minutes, 340 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07482452B2 |
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| 출처 데이터셋 | uspto-grants-2009_01 |
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| ORD ID | ord-2ee1d6d7c8e744f387b7fe51768a23ea |
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| 출처 메모 | uspto-grants-2009_01 |
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