関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | Methyl 2-thioxo-2,3-dihydrobenzoxazole-4-carboxylate | HCID 22272869 | — |
| 溶媒 | Phosphorus oxychloride | HCID 24813 | — |
| 生成物 | Methyl 2-chlorobenzo[d]oxazole-4-carboxylate | HCID 56924368 | 100.3% |
反応手順
A mixture of the thione from Step B (0.65 g, 3.11 mmol) and phosphorus pentachloride (0.65 g, 3.11 mmol) in phosphorus oxychloride (6 mL) was heated to 95° C. for 2.5 h. After cooling to room temperature, the reaction mixture was concentrated and dried on vacuum to give methyl 2-chlorobenzoxazole-4-carboxylate (0.66 g, quantitative) as a brown solid: 1H NMR (300 MHz, CDCl3) δ 8.05 (dd, J 8.1, 1.2 Hz, 1H), 7.72 (dd, J 8.1, 1.2 Hz, 1H), 7.45 (t, J=8.1 Hz, 1H), 4.04 (s, 3H); MS (ESI+) m/z 212 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07863271B2 |
|---|
| 出典データセット | uspto-grants-2011_01 |
|---|
| ORD ID | ord-2e994a9771c5421094e686623bff71a1 |
|---|
| 出典メモ | uspto-grants-2011_01 |
|---|
