化工社化工社 化学情報印刷レポート · 研究参考用
Cesium carbonate → 3-(3-Nitrophenylthio)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 3-Bromopyridine | HCID 12286 | — |
| 反応物 | Ethyl 2-oxocyclohexanecarboxylate | HCID 95543 | — |
| 反応物 | 3-Nitrobenzene-1-thiol | HCID 243576 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 3-(3-Nitrophenylthio)pyridine | HCID 118492332 | 43.1% |
反応手順
3-nitrophenylmercaptan (5 g, 32 mmol), 3-bromopyridine (6.1 g, 38.6 mmol), ethyl 2-oxocyclohexylformate (1.1 g, 6.5 mmol), copper iodide (608 mg, 4.2 mmol), cesium carbonate (2.3 g, 70.6 mmol) were dissolved in 500 ml of DMSO, reacted under microwaves at 100° C. for 8 h. After being extracted with water and DCM, the organic phase was dried and separated with column chromatography to obtain an object product 3.2 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09181244B1 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-a0d13f15a77e4ef9bae4bf6373c2ca64 |
| 出典メモ | uspto-grants-2015_11 |