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Water → 6-Methyl-2-nitrophenylpyruvic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,2-Dimethyl-3-nitrobenzene | HCID 6739 | — |
| 反応物 | Diethyl Oxalate | HCID 7268 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-Methyl-2-nitrophenylpyruvic acid | HCID 21194232 | 94.2% |
反応手順
Sodium metal (3.80 g, 165 mmol) was dissolved in absolute ethanol (66 mL) at 0° C. The 3-nitro-o-xylene (10 g, 66.2 mmol) and diethyl oxalate (18 mL, 132 mmol) were then added and the reaction was warmed to room temperature and stirred for 18 hours. The reaction was refluxed for 30 minutes, then cooled and water (22 mL) was added and the reaction was stirred at room temperature for one hour. The reaction was concentrated to remove the ethanol, then extracted with ethyl acetate, washed with brine, dried over sodium sulfate, filtered and concentrated to provide the desired product (13.92 g, 94%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06117885 |
| 出典データセット | uspto-grants-2000_09 |
| ORD ID | ord-99e359eefa6243b5908a714353b47a5f |
| 出典メモ | uspto-grants-2000_09 |