化工社化工社 化学情報印刷レポート · 研究参考用
2-Ethylphenylhydrazine Hydrochloride → 3-(4,6-Dimethoxypyrimidine-2-yl)-2-methyl-7-ethylindole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Ethylphenylhydrazine Hydrochloride | HCID 2733209 | — |
| 反応物 | 1-(4,6-Dimethoxypyrimidin-2-yl)propan-2-one | HCID 11264052 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-(4,6-Dimethoxypyrimidine-2-yl)-2-methyl-7-ethylindole | HCID 11335473 | 81.3% |
反応手順
Into a reactor were fed 2.4 g (12.2 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone, 1.7 g (9.98 m moles) of 2-ethylphenylhydrazine hydrochloride, 1.4 g (10.2 m moles) of zinc chloride and 10 ml of toluene, followed by refluxing for 2 hours with heating. After the completion of the reaction, the reaction mixture was cooled to room temperature. Thereto were added water and ethyl acetate and phase separation was made. The ethyl acetate layer was concentrated. The concentrate was subjected to silica gel column chromatography separation (developing solvent: n-hexane/ethyl acetate) to obtain 2.38 g (8.01 m moles) of 3-(4,6-dimethoxypyrimidine-2-yl)-2-methyl-7-ethylindole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07820861B2 |
| 出典データセット | uspto-grants-2010_10 |
| ORD ID | ord-70f244c9815f41ecb32f60b66997f436 |
| 出典メモ | uspto-grants-2010_10 |