関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Trifluoroacetic anhydride | HCID 9845 | — |
| 反応物 | 1-(1-(4-Chlorophenyl)cyclobutyl)-2-nitroethanol | HCID 66747669 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Chloro-4-{1-[(E)-2-nitroethenyl]cyclobutyl}benzene | HCID 66746852 | — |
反応手順
1-(1-(4-Chlorophenyl)cyclobutyl)-2-nitroethanol (5.2 g, 20.34 mmol) was dissolved in dichloromethane (41 ml) and trifluoroacetic acid anhydride (2.87 ml, 20.34 mmol) was added. The reaction mixture was cooled to 0° C. and triethylamine (5.67 ml, 40.7 mmol) was added dropwise. The reaction was slowly warmed to room temperature and stirring Was continued for 2 h. The reaction mixture was diluted with dichloromethane and washed with aqueous hydrochloric acid (1 N). The organic layer was dried (magnesium sulfate) and concentrated in vacuo. The crude product was purified by flash chromatography (silica, dichloromethane, methanol). Yield: 3.99 g (16.79 mmol, 83%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08877794B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-0d12ee125a564d98892a285f8e239deb |
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| 出典メモ | uspto-grants-2014_11 |
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