참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Bromobenzoic acid | HCID 6940 | — |
| 반응물 | 4-Nitroaniline | HCID 7475 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 2-bromo-N-(4-nitrophenyl)benzamide | HCID 5212555 | 87% |
반응 단계
Thionyl chloride (120.5 g) was added to a stirred mixture of 2-bromobenzoic acid (194 g) in toluene (500 ml) and N,N-dimethylformamide (DMF) (5 ml) and the mixture heated at 80° C. for 4 hours. The solution was cooled to 20° C. and added slowly to a solution of 4-nitroaniline (133.1 g) in toluene (500 ml) and NMP (120 ml), maintaining the temperature of the reaction mixture between 20°-25° C. The reaction mixture was then stirred for 24 hours when a solid precipitated. Water (360 ml) was added with rigorous stirring and the suspended solid collected by filtration, and washed successively with water, toluene and acetonitrile to give 2-bromo-N-(4-nitrophenyl)benzamide as a solid, in 87% yield, which was used without further purification or characterisation.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05245035 |
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| 출처 데이터셋 | uspto-grants-1993_09 |
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| ORD ID | ord-55c8dbdb7e544eb9a79fb8565a5af017 |
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| 출처 메모 | uspto-grants-1993_09 |
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