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 | 2-(Methoxymethoxy)benzaldehyde | HCID 10877485 | — |
| 生成物 | Methoxymethyl 2-(2-nitrovinyl)phenyl ether | HCID 131735043 | — |
反応手順
2-Methoxymethoxybenzaldehyde (16.4 g) was suspended in nitromethane (54 mL), added with ammonium acetate (5.95 g), and stirred for 30 minutes at 80° C. After cooling to room temperature, the solvent was evaporated under reduced pressure and the residue was suspended in water and then extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium hydrogen carbonate and saturated brine in order and dried over anhydrous sodium sulfate. The solvent was then evaporated under reduced pressure. The residues were purified by diol silica gel column chromatography (5% ethyl acetate/hexane) to obtain the title compound (11.6 g) as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09290440B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-7b8eb08023334a7e8fd968674c7f46bf |
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| 出典メモ | uspto-grants-2016_03 |
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