関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-(2,4-Dichlorophenyl)-3-hydroxyprop-2-enenitrile | HCID 1483069 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-(2,4-dichlorophenyl)-6-methyl-2(1H)-pyridone | HCID 18408325 | 45% |
反応手順
α-(2,4-dichlorophenyl)-α-hydroxymethylene acetonitrile and 8.8 g of acetone were thoroughly mixed with 110 g of polyphosphoric acid, and the mixture was heated to about 130° C. At this temperature, an exothermic reaction started. The temperature was maintained from 130 to 140° C. for 30 minutes, while heating as the case required. The cooled mixture was poured into ice water, and this suspension was stirred for 18 hours. This crude product was stirred with ethyl acetate and an excess amount of a dilute aqueous potassium hydroxide solution to make it alkaline. The formed precipitate was collected by filtration and washed sequentially with water, ethyl acetate and diethyl ether to obtain 8.0 g (yield: 45%) of the desired product. Melting point: 266-268° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06265349B1 |
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| 出典データセット | uspto-grants-2001_07 |
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| ORD ID | ord-84a3878e17584c83b2b6ef130b887074 |
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| 出典メモ | uspto-grants-2001_07 |
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