関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisobutylamine | HCID 8085 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Benzoic acid, 2,6-dinitro- | HCID 119206 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N,N-diisobutyl-2,6-dinitrobenzamide | HCID 21272460 | 64.8% |
反応手順
To a slurry of 106.5 g of 2,6-dinitrobenzoic acid in 1000 ml of toluene was added with stirring 133.2 g of diisobutylamine. Next 44.9 g of phosphorus oxychloride was added dropwise at such a rate to maintain the temperature below 40° C. The mixture was heated to 50° C. for 12 hrs and poured into 500 ml of aqueous 5% NaHCO3 solution with stirring. The organic layer was separated, washed with 500 ml water, and the toluene removed under reduced pressure. The remaining solid was recrystallized from hot ethanol to give 105.2 g of N,N-diisobutyl-2,6-dinitrobenzamide, a yellow solid, mp 97°-99° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04810769 |
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| 出典データセット | uspto-grants-1989_03 |
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| ORD ID | ord-2c7d3a4bb767437e821819555240276b |
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| 出典メモ | uspto-grants-1989_03 |
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