참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diisobutylamine | HCID 8085 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | Benzoic acid, 2,6-dinitro- | HCID 119206 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | N,N-diisobutyl-2,6-dinitrobenzamide | HCID 21272460 | 64.8% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04810769 |
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| 출처 데이터셋 | uspto-grants-1989_03 |
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| ORD ID | ord-2c7d3a4bb767437e821819555240276b |
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| 출처 메모 | uspto-grants-1989_03 |
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