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3-Methyl-4-nitrobenzyl alcohol → 3-Methyl-4-nitrobenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Methyl-4-nitrobenzyl alcohol | HCID 591360 | — |
| 反応物 | HCID 178418287 | HCID 178418287 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Methyl-4-nitrobenzaldehyde | HCID 11194528 | — |
反応手順
To a solution of (3-methyl-4-nitrophenyl)methanol (1.0 equiv.) in dichloromethane, pyridinium chlorochromate (1.1 equiv.) was added and the reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was filtered through celite and the filtrate was evaporated. The residue was adsorbed on silica (100-200 mesh) and purified by flash chromatography on silica gel, eluting with 5% ethyl acetate in petroleum ether (60-80), to provide the title compound in the form of creamish crystals (93%); 1H NMR (300 MHz, CDCl3) δ: 2.66 (s, 3H), 7.84-7.87 (m, 2H), 8.04-8.07 (d, J=8.7 Hz, 1H), 10.12 (s, 1H); IR (KBr) 3104, 3079, 2981, 2857, 2743, 1702, 1607, 1518, 1383, 1361, 1308, 1226, 1153, 1008, 832, 735 cm−1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835428B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-261ccf64a29d41a0a833c005d184fa3e |
| 出典メモ | uspto-grants-2014_09 |