化工社化工社 化学情報印刷レポート · 研究参考用
Methanol → 6-Methoxy-1-benzofuran-2-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Ethyl 6-methoxybenzofuran-2-carboxylate | HCID 11830962 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6-Methoxy-1-benzofuran-2-carboxylic acid | HCID 918863 | 91% |
反応手順
To a stirred solution of Product of Step B (0.25 g, 1.21 mmol) in a mixture of THF, MeOH and H2O (5 ml:2 ml:1 ml), LiOH (0.145 g, 6 mmol) in H2O (0.5 ml) was added and the mixture was stirred for 3 h at room temp. The solvents were distilled off and the residue was portioned between EtOAc (20 ml) and 1M HCl (2 ml). The organic layer was washed with H2O, dried over MgSO4 and filtered. The filtrate was evaporated to dryness to give the title compound (0.21 g, 91%), as a colourless solid. 1H-NMR (DMSO-d6) 7.61 (d, 1H, J=8.67 Hz); 7.54 (s, 1H); 7.24 (d, 1H, J=1.59 Hz); 6.93 (dd, 1H, J=8.67, 2.4 Hz); 3.8 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09193716B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-24371ff142734ca1a8a5b30910cd56a1 |
| 出典メモ | uspto-grants-2015_11 |