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Acetone → 4-(3-Ethoxy-4-hydroxyphenyl)but-3-en-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethylvanillin | HCID 8467 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(3-Ethoxy-4-hydroxyphenyl)but-3-en-2-one | HCID 69247429 | 70.4% |
反応手順
10% sodium hydroxide aqueous solution (80 ml) was added under stirring to a solution of 3-ethoxy-4-hydroxybenzaldehyde (16.6 g, 100 mmol) in acetone (50 ml), 95% ethanol (50 ml) and water (400 ml). The reaction mixture was stirred for 24 hr at room temperature, after the reaction completed, the reaction mixture was neutralized with 6N hydrochloric acid to adjust pH=7.0, the precipitated yellow solid was collected by filtration, washed with water and ethanol successively, dried, and then recrystallized from 95% ethanol to give 14.5 g of a yellow crystal, mp: 98-100° C., yield 70.4%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524744B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-ff7f346f666d4b05a119f33b618adecf |
| 出典メモ | uspto-grants-2013_09 |