化工社化工社 化学情報印刷レポート · 研究参考用
4-Toluenesulfonyl chloride → 2-Methyl-4-[(4-methylbenzenesulfonyl)oxy]butan-2-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | Isopentyldiol | HCID 247470 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Methyl-4-[(4-methylbenzenesulfonyl)oxy]butan-2-ol | HCID 14001295 | — |
反応手順
To a solution of 3-methylbutane-1,3-diol (2.5 mL) in dichloromethane (30 mL) and pyridine (2.1 mL) is added at 0° C. p-toluene-sulfonylchloride (4.6 g) in portions. The mixture is stirred for 12 hours at room temperature, diluted with dichloromethane and washed with 1 M aqueous HCl solution and brine. After drying (MgSO4) the solvent is evaporated and the product is purified by chromatography on silica gel (cyclohexane/ethyl acetate 90:10→70:30) to give the title compound. Yield: 3.2 g; Mass spectrum (ESI+): m/z=276 [M+NH4]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08642585B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-806d6d4232fe479eabfcec541b3fac8a |
| 出典メモ | uspto-grants-2014_02 |