化工社化工社 化学情報印刷レポート · 研究参考用
Water → 3-Ethyl-5-(5-chloro-6-methylthio-3-pyridyl)-isoxazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Nitropropane | HCID 7903 | — |
| 反応物 | 1,4-Diisocyanatobenzene | HCID 61009 | — |
| 反応物 | 3-Chloro-5-ethynyl-2-methylthiopyridine | HCID 23288266 | — |
| 触媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 3-Ethyl-5-(5-chloro-6-methylthio-3-pyridyl)-isoxazole | HCID 23288273 | 479.8% |
反応手順
A mixture of 3-chloro-5-ethynyl-2-methylthiopyridine (0.5 g, 2.72 mmol), 1-nitropropane (0.24 g, 0.27 mmol), 1,4-phenylenediisocyanate (1.3 g, 7.93 mmol) and triethylamine (5 drops) in benzene (20 mL) was heated under reflux with stirring for 8 hours, and allowed to stir at room temperature overnight. Water (1 mL) was added and the mixture stirred at room temperature for 2 hours. It was filtered through Celite, dried over anhydrous sodium sulphate and evaporated under reduced pressure. Recrystallisation of the residue from hexane gave the desired product (0.33 g, 48%) as a cream solid, melting point. 78-80° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06133294 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-fde49c4efa35456d916553572faf7e32 |
| 出典メモ | uspto-grants-2000_10 |