化工社化工社 化学情報印刷レポート · 研究参考用
Ammonia → 3-Anilino-4-methyl-6-oxo-7-phenyl-6,7-dihydrothieno[2,3-b]pyridine-2-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 1-Ethoxyethanol | HCID 10129898 | — |
| 反応物 | Ethyl 3-anilino-4-methyl-6-oxo-7-phenyl-6,7-dihydrothieno[2,3-b]pyridine-2-carboxylate | HCID 68457883 | — |
| 生成物 | 3-Anilino-4-methyl-6-oxo-7-phenyl-6,7-dihydrothieno[2,3-b]pyridine-2-carboxamide | HCID 68455219 | 66% |
反応手順
A mixture of Example 97 (150 mg, 0.37 mmol), ethoxyethanol and liquid ammonia was heated in a sealed vessel at 80° C. at 400 psi for 16 h. The mixture was concentrated in vacuo and the solid recrystallised from MeOH to give the title compound as a yellow solid (92 mg, 66%). δH (DMSO-d6) 8.05 (1H, s), 7.68-7.59 (3H, m), 7.53-7.51 (2H, m), 7.5 (1H, br), 7.24-7.20 (2H, m), 6.80 (1H, t, J 7.3 Hz), 6.64 (2H, d, J 7.7 Hz), 6.29 (1H, s), 2.22 (3H, s). LCMS (ES+) RT 3.074 minutes, 375.9 (M+H)+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07423047B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-fa79ce90a41c4918ad7a91e7cdec257e |
| 出典メモ | uspto-grants-2008_09 |