関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | Butylamine | HCID 8007 | — |
| 反応物 | 1-Nitrobutane | HCID 12302 | — |
| 反応物 | Methyl 4-Formylbenzoate | HCID 15294 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl 4-[(1Z)-2-nitropenta-1-enyl]benzoate | HCID 58807290 | 46.7% |
反応手順
n-Butylamine (8.31 ml, 84.1 mmol) and methyl 4-formylbenzoate (10.6 g, 64.7 mmol) was heated with reflux benzene (50 ml) in a Dean-Stark trap until a theoretical amount of water was recovered. The solvent was evaporated under reduced pressure. To the residue were added glacial acetic acid (30 ml) and nitrobutane (10.0 g, 97.0 mmol), and the mixture was stirred at 110° C. for 4 hrs. and allowed to cool to room temperature. The insoluble materials were filtered off and dried to give the title compound (7.53 g) as a pale-yellow powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07183415B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-55c2bf59c9ae48ebafa26b9b38aadab3 |
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| 出典メモ | uspto-grants-2007_02 |
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