関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | P-Anisidine | HCID 7732 | — |
| 反応物 | Methyl 3-amino-4-phenylthiophene-2-carboxylate | HCID 2759782 | — |
| 反応物 | Trimethylaluminum | HCID 16682925 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-Amino-N-(4-methoxyphenyl)-4-phenylthiophene-2-carboxamide | HCID 86729800 | 85.7% |
反応手順
p-Anisidine (29 mg, 0.24 mmol) was dissolved in toluene (2 ml) in a reaction vessel, and trimethylaluminum (2 M in TIIF, 0.12 ml) was added thereto at 0° C. After stirring for 10 min, to the mixture was added methyl 3-amino-4-phenylthiophene-2-carboxylate (50 mg, 0.21 mmol). The resulting mixture was heated to reflux at 120° C. for 16 hr. The completion of the reaction was confirmed by TLC. The reaction mixture was allowed to cool to room temperature, extracted with EtOAc, dried over anhydrous MgSO4, and concentrated under reduced pressure. The concentrate was purified by silica gel column chromatography (hexane:EtOAc=5:1) to give (57 mg, 0.18 mmol, 84% yield) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09260448B2 |
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| 出典データセット | uspto-grants-2016_02 |
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| ORD ID | ord-9d507646114648c5bd9f984a4ea6a178 |
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| 出典メモ | uspto-grants-2016_02 |
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