Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylethylamine → 2-Chloro-N-(3-iodo-4-methylphenyl)pyridine-4-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 3-Iodo-p-toluidine | HCID 118889 | — |
| 반응물 | 2-Chloroisonicotinic acid | HCID 236985 | — |
| 반응물 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Chloro-N-(3-iodo-4-methylphenyl)pyridine-4-carboxamide | HCID 21914557 | 89.5% |
반응 단계
2-Chloroisonicotinic acid (3.3 g, 21 mmol), HATU (8.75 g, 23 mmol), diisopropylethyl amine (10.9 ml, 63 mmol) and 3-iodo-4-methylaniline (5.00 g, 21 mmol) in dimethylformamide (50 ml) were heated under nitrogen for 16 hours. The reaction was cooled, solvent removed in vacuo and the residue taken up in dichloromethane (150 ml). The organic solution was washed with water (3×100 ml) and brine (100 ml), dried over magnesium sulfate, filtered and solvent removed in vacuo. The residue was purified by column chromatography (40:60 ethyl acetate:cyclohexane) to give 2-chloro-N-(3-iodo-4-methylphenyl)-isonicotinamide as a white solid (7.00 g, 18.8 mmol).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07425555B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-d4e6a59278a04225b468bb83eac89466 |
| 출처 메모 | uspto-grants-2008_09 |