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-(6-Methyl-pyridin-2-yloxymethyl)-benzaldehyde | HCID 59255148 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Methyl-6-(4-((E)-2-nitro-vinyl)-benzyloxy)-pyridine | HCID 59255368 | 110% |
反応手順
To a solution of 4-(6-methyl-pyridin-2-yloxymethyl)-benzaldehyde (4.19 g, 18.5 mmol) described in Manufacturing Example 3-1-2 in acetic acid (30 mL) were added nitromethane (5.65 g, 92.6 mmol) and ammonium acetate (2.85 g, 37.0 mmol) under nitrogen atmosphere, which was stirred for 3 hours at 110° C. The reaction mixture was partitioned into water and ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under a reduced pressure to obtain the title compound (5.50 g) as a crude product.
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-cdb111a9e34d42179f10e79e663164f2 |
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| 出典メモ | uspto-grants-2010_04 |
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