참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | 3-Chloropyridine-4-carboxylic acid | HCID 2735816 | — |
| 반응물 | 2-Amino-4-chloro-5-(trifluoromethyl)phenol | HCID 66880478 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-chloro-N-[5-chloro-2-hydroxy-4-trifluoromethylphenyl]isonicotinamide | HCID 66880791 | 69.9% |
반응 단계
A mixture of 0.60 g of 2-amino-4-chloro-5-trifluoromethylphenol, 0.43 g of 3-chloroisonicotinic acid, 0.67 g of WSC and 5 ml of pyridine was stirred while heating at 80° C. for three hours. The reaction mixture was cooled to room temperature, and then water was added, followed by extraction with ethyl acetate three times. The combined organic layers were washed with water and a saturated sodium chloride solution, dried anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 0.67 g of 3-chloro-N-[5-chloro-2-hydroxy-4-trifluoromethylphenyl]isonicotinamide.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08242133B2 |
|---|
| 출처 데이터셋 | uspto-grants-2012_08 |
|---|
| ORD ID | ord-729614d889394d2598aae2e6066655e1 |
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| 출처 메모 | uspto-grants-2012_08 |
|---|
