関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 5-Methoxy-2-nitrophenol | HCID 219635 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 生成物 | 2'-Hydroxy-4'-methoxyacetanilide | HCID 4105139 | 80% |
反応手順
2-Nitro-5-methoxyphenol (R. J. Maleski, Synthetic Communications, 23(3), 343-348 (1993)) (48.5 g, 0.287 mol) dissolved in tetrahydrofuran (THF) (1.5 L) was hydrogenated at ambient temperature over night with 10% Pd/C (10 g) until 20.3 L of hydrogen was consumed. After filtration and evaporation the residue was suspended in degased water (1.7 L) and acetic anhydride (42.5 mL) was added with stirring. The mixture was heated to 60° C. for 1 h and then cooled. The isolated solid was washed thoroughly with water and dried in vacuo to give brick-red crystals (41.7 g, 80%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07388020B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-5b5ec7be27b84bcf93823c6d02e5c47e |
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| 出典メモ | uspto-grants-2008_06 |
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