関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4'-Hydroxypropiophenone | HCID 6271 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Benzylpyridine | HCID 16458 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Platinum oxide (PtO) | HCID 82844 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Ifenprodil | HCID 3689 | 92.3% |
反応手順
To 4 ml of dioxane were added 6.0 g of 4'-hydroxypropiophenone. 6.8 Grams of bromine were added dropwise to the mixture with stirring at room temperature, and the reaction liquid was stirred for an additional 10 minutes. To the reaction liquid were then added 7.5 g of 4-benzylpyridine, 2.1 g of potassium carbonate, 1 ml of water and 50 ml of methanol, and the mixture was refluxed under heating for 5 hours. After stopping the heating, 25 ml of methanol and 0.2 g of platinum oxide were added and hydrogen was then introduced and the mixture was stirred for 8 hours under pressure of about 1 atm. After completion of the reaction, the reaction mixture was worked up in the same manner as described in Example 46, whereby 12.0 g (77.9%) of ifenprodil were obtained as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04377691 |
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| 出典データセット | uspto-grants-1983_03 |
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| ORD ID | ord-e9719236f7bd46719c424a3bcb53e5af |
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| 出典メモ | uspto-grants-1983_03 |
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