関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cinnamoylbenzene | HCID 7189 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(Carbamoylmethyl)pyridinium Chloride | HCID 2756440 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4,6-Diphenyl-2-pyridone | HCID 3846201 | — |
反応手順
To a solution of benzylideneacetophenone (41.6 g) and N-carbamoylmethylpyridinium chloride (34.4 g) (prepared according to the method of O. ALBRECHT et al., Helv. Chim. Acta 24, 241E (1941)) in methanol (600 cc), is added, at room temperature, a 1N aqueous solution of sodium hydroxide (200 cc). The initially yellow solution takes on an orange colour and a yellow solid precipitates. The mixture is stirred at room temperature for 15 minutes and acetic acid (400 cc) is then added. The green solution obtained is stirred for 1 hour at room temperature. The solvent is then distilled in 4 hours under atmospheric pressure. The solid residue obtained is taken up in distilled water (500 cc). After stirring for 1 hour at more temperature, the solid is separated by filtration, washed with distilled water (3×100 cc) and dried under reduced pressure at 60° C. (whitish solid; m.p.=209°-212° C.)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05366982 |
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| 出典データセット | uspto-grants-1994_11 |
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| ORD ID | ord-5319b62429fc474e93ef5a19e3e0c3bd |
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| 出典メモ | uspto-grants-1994_11 |
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