関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Anisole | HCID 7519 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | 3-Trifluoromethyl-5-trifluoromethanesulfonyl-1,2,4-triazole | HCID 178527382 | — |
| 触媒 | Scandium | HCID 23952 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Nitromethane | HCID 6375 | — |
| 生成物 | 4'-Methoxyacetophenone | HCID 7476 | 97.2% |
反応手順
The catalytic effect of the scandium salt of 3-trifluoromethyl-5-trifluoromethanesulfonyl-1,2,4-triazole, obtained in Example 3, relative to a reaction was evaluated in the following manner. In 40 ml of anhydrous nitromethane, there is added 592 mg (700 μmoles) of the scandium salt of 3-trifluoromethyl-5-trifluoromethanesulfonyl-1,2,4-triazole, and 1.08 g (10 mmoles) of anisol and 2.04 g of acetic anhydride. After stirring during 10 min at 21° C., the reaction mixture was diluted with 50 ml of ether and the reaction was inhibited by 100 ml of a saturated solution of sodium bicarbonate NaHCO3. After filtration on Celite, the solution was extracted with three fractions of 50 ml ether, and the collected ether phase was washed with a saturated solution of potassium chloride. After drying the ether phase with magnesium sulfate and evaporation, 1.46 g of p-methoxyacetophenone (97% yield) was collected, with a purity characterized by a proton RMN higher than 99%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06395367B1 |
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| 出典データセット | uspto-grants-2002_05 |
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| ORD ID | ord-844711d13716471f999b8846d1e7f3b3 |
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| 出典メモ | uspto-grants-2002_05 |
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