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Water → 3-(4,6-Dimethoxypyrimidine-2-yl)-2-methylindole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phenylhydrazine | HCID 7516 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 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-methylindole | HCID 12979368 | 62% |
反応手順
In 10 ml of toluene were dissolved 1.61 g (8.2 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone and 1.08 g (10 m moles) of phenylhydrazine. Thereto was added 1.36 g (10 m moles) of zinc chloride, followed by refluxing for 1 hour. The reaction mixture was allowed to cool, and ethyl acetate and water were added to dissolve the whole reaction mixture. The oily layer was washed with water, separated and dried over Glauber's salt. The resulting oily layer was concentrated under reduced pressure to obtain an orange solid. The solid was recrystallized from methanol to obtain 1.37 g (5.1 m moles) of 3-(4,6-dimethoxypyrimidine-2-yl)-2-methylindole. Yield: 62% Melting point: 182 to 184° C.
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-4af464b6fbdb416b831efb491e917bd8 |
| 出典メモ | uspto-grants-2010_10 |