참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | 2-Amino-5-bromopyridine | HCID 70622 | — |
| 반응물 | 3,4,5-Trimethoxy-2-nitrobenzoic acid | HCID 97116 | — |
| 촉매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | n-(5-Bromo(2-pyridyl))(3,4,5-trimethoxy-2-nitrophenyl)carboxamide | HCID 22596319 | 98.3% |
반응 단계
To a solution of 3,4,5-trimethoxy-2-nitrobenzoic acid (0.5 g, 1.95 mmol) in dichloromethane (5 ml) was added oxalyl chloride (0.34 ml, 3.9 mmol) and a few drops of dimethylformamide. The mixture was stirred at r.t. for 2 hrs. After the evaporation of the solvent, the residue was dissolved in dichloromethane (5 ml). 2-amino-5-bromopyridine (0.81 g, 4.7 mmol) and pyridine (0.94 ml, 11.7 mmol) were added to the solution. The mixture was stirred at r.t. overnight. After the evaporation of the solvent, the crude residue was purified by silica gel column chromatography using solvent system 25% ethyl acetate in hexane as eluent to give N-(5-bromo(2-pyridyl))(3,4,5-trimethoxy-2-nitrophenyl)carboxamide as a solid (790 mg, 98%). MS found for C15H14BrN3O6 M+=412, (M+2)+=414.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09108922B2 |
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| 출처 데이터셋 | uspto-grants-2015_08 |
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| ORD ID | ord-dab9550dd4164c2db31d42a0d8c82895 |
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| 출처 메모 | uspto-grants-2015_08 |
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