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3-(2-Thienyl)-5-isoxazolamine → Ethyl 6-(5-methylpyridin-3-yl)-3-(thiophen-2-yl)isoxazolo[5,4-b]pyridine-4-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-(2-Thienyl)-5-isoxazolamine | HCID 216901 | — |
| 反応物 | HCID 178473093 | HCID 178473093 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Ethyl 6-(5-methylpyridin-3-yl)-3-(thiophen-2-yl)isoxazolo[5,4-b]pyridine-4-carboxylate | HCID 117844821 | — |
反応手順
A mixture of 1-3 (150 mg, 0.638 mmol) and 1-4 (106 mg, 0.638 mmol) in acetic acid (3 mL) was heated at reflux for 3 h. The mixture was cooled to rt and concentrated. The residue was purified by column chromatography (0-100% EtOAc in hexane) to give 1-5 as a white solid: 1H NMR (400 MHz, CDCl3) δ 9.16 (s, 1H), 8.59 (s, 1H), 8.36 (s, 1H), 8.15 (s, 1H), 7.58 (m, 1H), 7.39 (m, 1H), 7.22 (m, 1H), 4.21 (q, J=7.2 Hz, 2H), 2.48 (s, 3H), 1.07 (t, J=7.2 Hz, 3H); ESI+ MS [M+H]+ C19H16N3O3S=366.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09242995B2 |
| 出典データセット | uspto-grants-2016_01 |
| ORD ID | ord-bde9b82a95d14c6ab68c8973497111c4 |
| 出典メモ | uspto-grants-2016_01 |