関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Methyl vinyl ketone | HCID 6570 | — |
| 反応物 | m-Toluidine | HCID 7934 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4,7-Dimethylquinoline | HCID 123499 | — |
反応手順
A solution of 3-methyl-phenylamine (1 eq), in 1,4-dioxane is stirred and cooled to approximately 12° C. Sulfuric acid (2 eq.) is slowly added and heated at reflux. Methylvinyl ketone (1.5 eq) is added dropwise into the refluxing solution. The solution is heated for 1 h after addition is complete. The reaction solution is evaporated to dryness and dissolved in methylene chloride. The solution is adjusted to pH 8 with 1 M sodium carbonate and extracted with three times with water. The residue is chromatographed on SiO2 (70/30 hexane/ethylacetate) to yield the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07087626B2 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-da6e96936d2f4a35966ec382e248cadc |
|---|
| 出典メモ | uspto-grants-2006_08 |
|---|
