関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperonal | HCID 8438 | — |
| 反応物 | 3,4-Dimethoxyphenyl methyl ketone | HCID 14328 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3',4'-Dimethoxy-3,4-methylenedioxychalcone | HCID 291728 | 100.2% |
反応手順
To a warm (40° C.) solution of 41.5 grams (0.23 mole) of 3,4-dimethoxyacetophenone and 40.5 grams (0.27 mole) of piperonal in 220 milliliters of ethanol was added 60 milliliters of 10 % aqueous sodium hydroxide. The mixture was warmed for 10 minutes at 40°-50° C; then stirred at room temperature for 2 hours. After standing overnight, the yellow crystalline produce was collected by filtration, washed with water (3 × 40 milliliters), and dried to give 72 grams (quantitative yield) of V, melting point 127°-129° c. An analytical sample was prepared by recrystallization of 1.6 gram of the product from 50 milliliters of ethanol, giving 1.4 gram of pure chalcone as yellow needles, melting point 131°-133° C.; λ (ethanol) 242 (log ε 4.23), 3.60 nm (4.53).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04014885 |
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| 出典データセット | uspto-grants-1977_03 |
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| ORD ID | ord-404aec80e95c4e4bb125806d48fa82e6 |
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| 出典メモ | uspto-grants-1977_03 |
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