関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Chloro-3-methyl-2-butene | HCID 10429 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2',4',6'-Trihydroxyacetophenone | HCID 68073 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethanone, 1-[2,4,6-trihydroxy-3-(3-methyl-2-butenyl)phenyl]- | HCID 11687311 | 55% |
反応手順
In 250 ml of anhydrous tetrahydrofuran was dissolved 50.0 g of 2',4',6'-trihydroxyacetophenone, and 123.1 g of anhydrous potassium carbonate was added to the solution and the mixture was stirred at room temperature for 30 minutes. Then, 37.2 g of 1-chloro3-methyl-2-butene was added dropwise to the mixture over a period of 20 minutes and reaction was carried out at room temperature for 24 hours. After the reaction, the reaction mixture was extracted with 2 l of ethyl acetate and the solvent was removed from the ethyl acetate layer by distillation, and the residue was recrystallized from a benzene/petroleum ether mixed solvent to obtain 38.6 g (yield=55.0%) of 2',4',6'-trihydroxy-3'-(3-methyl-2-butenyl)acetophenone in the form of a yellow prism.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05106871 |
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| 出典データセット | uspto-grants-1992_04 |
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| ORD ID | ord-74e2a1ebf3ec4cde92c5887a9a38f149 |
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| 出典メモ | uspto-grants-1992_04 |
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