関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 2-Propynoic acid, 3-phenyl-, ethyl ester | HCID 91516 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | N-(4-fluorophenyl)-1-phenylpropaneimine | HCID 14726141 | — |
| 生成物 | 1-(4-fluorophenyl)-3-methyl-2,6-diphenyl-4(1H)-pyridinone | HCID 14303555 | — |
反応手順
To 300 ml of toluene were added 9.1 g (0.040 mole) of N-(4-fluorophenyl)-1-phenylpropaneimine, 4.7 g (0.035 mole) of aluminum chloride and 5.2 g (0.030 mole) of ethyl phenylpropiolate, followed by refluxing the resultant mixture for 5 hours. Thereafter, the reaction mixture was poured into 500 ml of 2N sulfuric acid which had been ice-cooled, followed by extraction with chloroform. After washing the organic layer with water, the organic layer wad dried over anhydrous sodium sulfate. Subsequent to removal of the sodium sulfate, the solvent was distilled off and the residue was purified by chromatography on a silica gel column (eluent: 1:50 mixed solvent of methanol and chloroform). The resultant crystals were recrystallized from a 1:1 mixed solvent of acetone and hexane to give 1.0 g of 1-(4-fluorophenyl)-3-methyl-2,6-diphenyl-4(1H)-pyridinone having a melting point of 256°-259° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04757081 |
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| 出典データセット | uspto-grants-1988_07 |
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| ORD ID | ord-3004a3c027a243cea900b2bf096adce4 |
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| 出典メモ | uspto-grants-1988_07 |
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