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Pyridine → 6-Phenyl-2-pyridone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Ethyl chloroacetate | HCID 7751 | — |
| 反応物 | 1-Propanone, 3-(dimethylamino)-1-phenyl-, hydrochloride (1:1) | HCID 92844 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-Phenyl-2-pyridone | HCID 87889 | — |
反応手順
Ethyl 2-chloroacetate (10.6 ml, 0.1 mol) is slowly added to hot (105° C.) pyridine (8.9 ml, 0.11 mol whereby the temperature is maintained in the range of 100° C. to 110° C. The resulting brown oil is dissolved in ethanol (60 ml), β-dimethylamino propiophenone hydrochloride (17.7 g, 0.1 mol; prepared according to Example 1) and ammonium acetate (60 g) are added and the mixture is boiled under reflux for 4 h. After cooling, the mixture is filtered and the solvent is evaporated in vacuo. The residue is crystallized from water, collected by filtration and purified by re-crystallization from toluene. The title compound is obtained as colorless crystals (4.7 g, 28% of th.) with mp. 200° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06008161 |
| 出典データセット | uspto-grants-1999_12 |
| ORD ID | ord-e8da0674e3194f368a28a8a48700cacb |
| 出典メモ | uspto-grants-1999_12 |