関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Hexamethylenetetramine | HCID 4101 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 1-Methoxy-4-(trifluoromethoxy)benzene | HCID 2724973 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | 2-Methoxy-5-(trifluoromethoxy)benzaldehyde | HCID 2783364 | — |
反応手順
Combine 2-methoxy-5-trifluoromethoxybenzene (1.0 g, 5.2 mmol) and trifluoroacetic acid (200 mL). Add slowly portionwise hexamethylenetetraamine (26 g, 185.7 mmol). Heat at 60° C. After 24 hours, cool to ambient temperature and pour the reaction mixture into a 2 M aqueous solution of sulfuric acid (500 mL). Cool and extract ten times with diethyl ether. Dry the combined organic layers over Na2SO4, filter, and evaporate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with 1/4 ethyl acetate/hexane to give 2-methoxy-5-trifluoromethoxybenzaldehyde.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05998439 |
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| 出典データセット | uspto-grants-1999_12 |
|---|
| ORD ID | ord-0dab936c8a554a56ae5ba95edab08a03 |
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| 出典メモ | uspto-grants-1999_12 |
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