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p-Toluenesulfonic acid → 4-(1,3-Thiazol-2-yl)phenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 2-Bromo-1,1-dimethoxyethane | HCID 81672 | — |
| 反応物 | 4-Hydroxythiobenzamide | HCID 2759344 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(1,3-Thiazol-2-yl)phenol | HCID 223840 | — |
反応手順
To a mixture of 4-hydroxybenzothioamide (30.64 g, 0.20 mol) and 2-bromo-1,1-dimethoxyethane (31.00 g, 0.20 mol) in EtOH (600 mL) was added 4-methylbenzenesulfonic acid (34.44 g, 0.20 mol) with stirring at rt. The reaction mixture was heated at 90° C. for 24 h, then cooled to rt and concentrated in vacuo. The mixture was diluted with H2O (200 mL), adjusted to pH 10 with saturated NaHCO3 aqueous solution and extracted with DCM (200 mL×3). The combined organic phases were concentrated in vacuo to give the title compound as s yellow solid (21.3 g, 60%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434695B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-18f547aa7dbd4e959f7a411db9b1cb6c |
| 出典メモ | uspto-grants-2016_09 |