化工社化工社 化学情報印刷レポート · 研究参考用
Hexane → 2-Methyl-6-(piperidine-1-sulfonyl)-benzothiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 2-Methyl-1,3-benzothiazole-6-sulfonyl chloride | HCID 3583019 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Methyl-6-(piperidine-1-sulfonyl)-benzothiazole | HCID 1075675 | 74.2% |
反応手順
A solution of Compound 2 (2.5 g, 10 mmol) in chloroform (15 ml) was added drop wise to a solution of piperidine (1.7 g, 20.0 mmol) in chloroform (10 ml). The combined mixture was stirred at room temperature for 1 hour. The reaction mixture was then washed with water (2×, 50 ml) and brine (1×, 50 ml). The organic layer was dried with sodium sulfate and evaporated. The sticky white solid thus obtained was dissolved in ca. 5 ml of hot ethyl acetate and this solution was then slowly added to 40 ml hexane. The white solid that precipitated was collected, washed with hexane and dried to yield 2.2 g (74%) of Compound 3, Rf=0.28 (30% ethyl acetate in hexane). The structure of Compound 3 is given below:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08759526B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-5e3b8c719ad04582899ed8877fe21f51 |
| 出典メモ | uspto-grants-2014_06 |