関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | o-Tolylhydrazinium(1+) chloride | HCID 71554 | — |
| 反応物 | 1-(4,6-Dimethoxypyrimidin-2-yl)propan-2-one | HCID 11264052 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | 3-(4,6-Dimethoxypyrimidine-2-yl)-2,7-dimethylindole | HCID 12979370 | 34.2% |
反応手順
In 20 ml of toluene were dissolved 0.77 g (3.9 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone and 0.69 g (4.3 m moles) of 2-methylphenylhydrazine hydrochloride. Thereto was added 0.64 g (4.7 m moles) of zinc chloride, followed by refluxing for 2 hours. The reaction mixture was allowed to cool, and then 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 using a rotary evaporator, to obtain an orange solid. The solid was treated with ethyl acetate/n-hexane to obtain 0.38 g (1.34 m moles) of 3-(4,6-dimethoxypyrimidine-2-yl)-2,7-dimethylindole. Yield: 34% Melting point: 145 to 147° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07521555B2 |
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| 出典データセット | uspto-grants-2009_04 |
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| ORD ID | ord-c0ad930bfbef403fb64ec853dfd4cffd |
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| 出典メモ | uspto-grants-2009_04 |
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