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 | 4-(Pyridin-2-ylmethoxy)benzaldehyde | HCID 759667 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-(4-((E)-Nitro-vinyl)-phenoxymethyl)-pyridine | HCID 59255195 | 97.3% |
反応手順
A mixture of 4-(pyridin-2-ylmethoxy)-benzaldehyde (29 g, 136 mmol) described in Manufacturing Example 203-1-1, nitromethane (36.6 mL, 680 mmol), ammonium acetate (21 g, 272 mmol), and acetic acid (300 mL) was stirred for 21 hours at 100° C. This mixture was cooled to room temperature and concentrated under a reduced pressure. The residue was partitioned into ethyl acetate and water. The organic layer was separated, washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure to obtain the title compound (33.9 g, 97%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07691882B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-908afebde5b3447283528a5f13508498 |
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| 出典メモ | uspto-grants-2010_04 |
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