化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → HCID 178448482、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Fluoro-5-(trifluoromethyl)benzoyl Chloride | HCID 2734880 | — |
| 反応物 | 3-(but-3-ynyl)-5-tert-butylthiazol-2(3H)-imine p-toluenesulfonate | HCID 86644542 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178448482 | HCID 178448482 | 91.9% |
反応手順
A mixture of 3-(but-3-ynyl)-5-tert-butylthiazol-2(3H)-imine p-toluenesulfonate (prepared as described in US20080242654) (2.6 g, 6.83 mmol) and 2-fluoro-5-(trifluoromethyl)benzoyl chloride (1.55 g, 6.83 mmol) in anhydrous CH2Cl2 (30 mL) was treated dropwise at 0° C. with triethylamine (1.91 mL, 1.38 mmol). The mixture was allowed to warm to room temperature and stirred for 14 hours. The mixture was then washed with water, brine, dried with MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by silica gel chromatography and eluted with hexane-EtOAc (2:1) to afford 2.5 g of the title compound. MS (DCI/NH3) m/z 399 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08895592B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-fa000a7de4b846c38da818ad1adff5b8 |
| 出典メモ | uspto-grants-2014_11 |