関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | 2'-Aminoacetophenone | HCID 11086 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Ethyl bromophenylacetate | HCID 97780 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (2-Acetyl-phenylamino)-phenyl-acetic acid ethyl ester | HCID 59401176 | 100.3% |
反応手順
1-(2-Aminophenyl)ethanone (250 mg, 1.85 mmol), ethyl 2-bromo-2-phenylacetate (0.22 ml, 1.23 mmol), DIPEA (0.32 mL, 1.85 mmol) and a catalytic amount of potassium iodide are dissolved in acetonitrile (4 mL) and heated under MW irradiation at 100° C. for 2 hours and then at 120° C. for 1 hour. Acetonitrile is evaporated and the crude is purified by flash chromatography (petroleum ether/EtOAc=93/7) to obtain intermediate I110 as a yellow oil (367 mg, quantitative yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08835682B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-5b91be84d1ed4518a37485df7db91f75 |
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| 出典メモ | uspto-grants-2014_09 |
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