참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Chloroacetonitrile | HCID 7856 | — |
| 반응물 | Sodium 1-(2-chlorophenyl)-3-cyano-6-oxo-1,6-dihydropyridine-2-thiolate | HCID 68805809 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-Amino-7-(2-chlorophenyl)-6-oxo-6,7-dihydrothieno[2,3-b]pyridine-2-carbonitrile | HCID 66970528 | 33.5% |
반응 단계
Chloroacetonitrile (0.35 mL, 5.5 mmol) was added to a solution of Example 2 (1.42 g, 5.0 mmol) in MeCN (50 mL) and the mixture heated at 40° C. for 3 h. H2O (100 mL) was added and the mixture concentrated in vacuo to remove some of the MeCN (remaining volume ˜120 mL). The mixture was cooled to 0° C. and the solid filtered off, washed with H2O (15 mL) and Et2O (2×15 mL) and dried to give the title compound as a pale brown solid (505 mg, 32%). δH (DMSO-d6) 8.10 (1H, d, J 9.7 Hz), 7.75-7.73 (1H, m), 7.65-7.54 (3H, m), 7.14 (2H, br s, NH2), 6.54 (1H, d, J 9.7 Hz). LCMS (ES+) RT 2.97 minutes, 302 (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-9e5e167e15994ecb8bf054adb72021fa |
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| 출처 메모 | uspto-grants-2009_01 |
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