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Water → N-(2-Methoxy-6-nitrophenyl)valeroamide
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 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 6-Nitro-o-anisidine | HCID 85491 | — |
| 溶媒 | Valeric anhydride | HCID 74959 | — |
| 生成物 | N-(2-Methoxy-6-nitrophenyl)valeroamide | HCID 19792196 | 36% |
反応手順
To a mixture of 2-methoxy-6-nitroaniline (5.9 g) in valeric anhydride (14 g) was added a catalytic amount of conc. sulfuric acid, which was stirred for 1.5 hour at 130°-140° C. To the reaction mixture was added water, which was made basic with 6N NaOH. The reaction mixture was extracted with ethyl acetate. The organic layer was washed with water and dried. The solvent was distilled off. The residue was purified by column chromatography on silica gel. Crude crystals thus obtained were recrystallized from ethyl acetate-hexane to give colorless crystals (3.2 g, 36%), m.p. 113°-114° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05128356 |
| 出典データセット | uspto-grants-1992_07 |
| ORD ID | ord-c0fd67846f7542e49c8920a16b2d71e3 |
| 出典メモ | uspto-grants-1992_07 |