関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitromethane | HCID 6375 | — |
| 反応物 | 4-Butoxybenzaldehyde | HCID 79813 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-Butoxy-4-((E)-2-nitro-vinyl)-benzene | HCID 6267903 | 76% |
反応手順
A mixture of 4-butoxy-benzaldehyde (4.72 g, 26.5 mmol) described in Manufacturing Example 67-1-1, nitromethane (2.85 mL, 53 mmol), ammonium acetate (3.06 g, 39.8 mmol) and acetic acid (40 mL) was stirred for 13 hours at 100° C. This mixture was cooled to room temperature, concentrated under a reduced pressure, and diluted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by silica gel column chromatography (heptane:ethyl acetate=4:1-1:1) to obtain the title compound (4.44 g, 76%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841327B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-b967ff8d1d954a9fbb72e99a5a4b2299 |
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| 出典メモ | uspto-grants-2014_09 |
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