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 | Hydrazine, (4-chlorophenyl)-, hydrochloride (1:1) | HCID 71600 | — |
| 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 | 5-Chloro-3-(4,6-dimethoxypyrimidine-2-yl)-2-methylindole | HCID 17856766 | 84% |
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 7.9 g (44 m moles) of 4-chlorophenylhydrazine hydrochloride. Thereto was added 6.54 g (48 m moles) of zinc chloride. Refluxing was made for 2 hours with heating. The reaction mixture was allowed to cool. Then, ethyl acetate and water were added to dissolve the whole reaction mixture. The organic layer was washed with water, separated, and dried over Glauber's salt. The resulting organic layer was concentrated under reduced pressure using a rotary evaporator to obtain an orange solid. The solid was washed with isopropyl ether to obtain 10.2 g (33.7 m moles) of 5-chloro-3-(4,6-dimethoxypyrimidine-2-yl)-2-methylindole. Yield: 84% Melting point: 179 to 181° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07531654B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-ead58d8be5a34a75b626e3cf4bce05b5 |
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| 出典メモ | uspto-grants-2009_05 |
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