関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 2,4-Dinitrobenzoic acid | HCID 11880 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Morpholine, 4-(2,4-dinitrophenylbenzoyl)- | HCID 544864 | 81.2% |
反応手順
To a slurry of 215.1 g of 2.4-dinitrobenzoic acid in 1000 ml of toluene was added with stirring 196.2 g of morpholine. Next 76.5 g of phosphorus oxychloride was added dropwise at such a rate to maintain the reaction temperature below 90° C. The mixture was refluxed for 5 hrs, cooled to 80° C., and slowly poured into 1000 ml of aqueous 5% NaHCO3 solution with stirring. The precipitate was filtered, washed with water and dried to yield 231.7 g of N-(2,4-dinitrobenzoyl)morpholine, mp 159°-161° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04937306 |
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| 出典データセット | uspto-grants-1990_06 |
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| ORD ID | ord-0ea86c4a16fd443e8ba7ef867682abe7 |
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| 出典メモ | uspto-grants-1990_06 |
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