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Water → 2,4-Dimethyl-5-nitroaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Acetamide, N-(2,4-dimethyl-5-nitrophenyl)- | HCID 112848 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2,4-Dimethyl-5-nitroaniline | HCID 228007 | — |
反応手順
A mixture of N-(2,4-dimethyl-5-nitrophenyl)acetamide, water (24 mL), concentrated sulfuric acid (12 mL), and ethanol (120 mL) was heated at reflux under an atmosphere of nitrogen for 4 hours. The ethanol was evaporated under reduced pressure and the residue partitioned between ethyl acetate (250 mL) and brine (150 mL). The brine solution was reextracted with ethyl acetate. The combined ethyl acetate extracts were then dried over magnesium sulfate. Evaporation afforded a crude product which was flash chromatographed on silica and eluted with ethyl acetate:hexane (1:4) to afford 4.63 g as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06057349 |
| 出典データセット | uspto-grants-2000_05 |
| ORD ID | ord-d80351a3127f41bc8ba186ed2b51f89f |
| 出典メモ | uspto-grants-2000_05 |