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 | 3-(Pyridin-2-ylmethoxy)benzaldehyde | HCID 6483805 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-(3-((E)-2-nitro-vinyl)-phenoxymethyl)-pyridine | HCID 59255249 | 71.4% |
反応手順
A mixture of 3-(pyridin-2-ylmethoxy)-benzaldehyde (2.98 g, 14 mmol) described in Manufacturing Example 60-1-1, nitromethane (1.51 mL, 28 mmol), ammonium acetate (1.62 g, 21 mmol) and acetic acid (30 mL) was stirred for 6 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, 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=4:1-2:1-1:1) to obtain the title compound (2.56 g, 71%).
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-320a051a5f1243e4b9c52dd49a11aefc |
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| 出典メモ | uspto-grants-2014_09 |
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