関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4'-Hydroxypropiophenone | HCID 6271 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 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 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Ifenprodil | HCID 3689 | 88.4% |
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 5 minutes. To the reaction liquid were then added 7.5 g of 4-benzylpyridine, 2.8 ml of 10-N sodium hydroxide solution and 100 ml of methanol, and the mixture was refluxed under heating for 5 hours. After stopping the heating, 0.5 g of platinum oxide were added and hydrogen was then introduced and the mixture was stirred for 7 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 11.5 g (74.7%) 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-ba1be67b37fd4f2b8a03023baa06c57f |
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| 出典メモ | uspto-grants-1983_03 |
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