化工社化工社 化学情報印刷レポート · 研究参考用
Ethylene Glycol → 2-Amino-5-methylbenzene-1-thiol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-Amino-6-methylbenzothiazole | HCID 17335 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Amino-5-methylbenzene-1-thiol | HCID 323260 | 87.3% |
反応手順
A mixture of 2-amino-6-methylbenzothiazole (15 g, 91.3 mmol), ethylene glycol (22.26 g, 0.36 mol) and 50% w/v KOH (180 ml) was heated under reflux for 62 h. On cooling to room temperature, toluene (60 ml) was added and the reaction mixture was cooled in an ice-bath and acidified with acetic acid (final pH 5-6). The reaction mixture was extracted with toluene (5×300 ml) and the combined organic extracts were washed with brine (2×200 ml), dried (MgSO4) and the solvent removed under reduced pressure to give the title compound (11.1 g, 86%) as a yellow solid which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08895313B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-3fddf22e12cf4bc68ed7a1a09f836cac |
| 出典メモ | uspto-grants-2014_11 |