化工社化工社 化学情報印刷レポート · 研究参考用
Toluene → 3-(4,6-Dimethoxypyrimidine-2-yl)-5-methoxy-2-methylindole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 4-Methoxyphenylhydrazine hydrochloride | HCID 2723904 | — |
| 反応物 | 1-(4,6-Dimethoxypyrimidin-2-yl)propan-2-one | HCID 11264052 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(4,6-Dimethoxypyrimidine-2-yl)-5-methoxy-2-methylindole | HCID 17856763 | 67% |
反応手順
To 80 ml of toluene were added 8.0 g (40 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone and 7.7 g (44 m moles) of 4-metoxyphenylhydrazine hydrochloride. Thereto was added 6.0 g (44 m moles) of zinc chloride. Refluxing was made for 2 hours with heating. The reaction mixture was allowed to cool. Thereto were added ethyl acetate and water to dissolve the whole reaction mixture. The oily layer was washed with water, separated and dried over Glauber's salt. The resulting organic layer was concentrated under reduced pressure using an rotary evaporator to obtain, as an orange solid, 8.0 g (26.7 m moles) of 3-(4,6-dimethoxypyrimidine-2-yl)-5-methoxy-2-methylindole. Yield: 67% Recrystallization from toluene was made.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07531654B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-f874ce1897784008bb6ea42e66a46d75 |
| 出典メモ | uspto-grants-2009_05 |