関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitromethane | HCID 6375 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | 6-Benzyl-pyridine-3-carbaldehyde | HCID 21698347 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Benzyl-5-((E)-2-nitro-vinyl)-pyridine | HCID 59255390 | 21% |
反応手順
A mixture of 6-benzyl-pyridine-3-carbaldehyde (4.7 g, 24 mmol) described in Manufacturing Example 210-1-4, nitromethane (7.3 g, 120 mmol), ammonium acetate (5.6 g, 72 mmol), and acetic acid (40 mL) was stirred for 90 minutes at 100° C. The reaction solution was partitioned into ethyl acetate and water. The organic layer was washed with saturated aqueous sodium bicarbonate and concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (heptane:ethyl acetate=2:1) to obtain the title compound (1.2 g, 21%).
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-915bcabfd56045e0ad69d903bca137a3 |
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| 出典メモ | uspto-grants-2014_09 |
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