Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
N-Methylbutylamine → Methyl 3-{[butyl(methyl)amino]carbonyl)-5-iodobenzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | N-Methylbutylamine | HCID 8068 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 반응물 | 3-Iodo-5-(methoxycarbonyl)benzoic acid | HCID 15840391 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Methyl 3-{[butyl(methyl)amino]carbonyl)-5-iodobenzoate | HCID 21086165 | — |
반응 단계
3-Iodo-5-(methoxycarbonyl)benzoic acid (1 g, 3.3 mmol) is dissolved in DMF (10 mL), and diisopropylethylamine (1.7 mL, 9.8 mmol), HATU (1.5 g, 3.9 mmol), and N-methylbutylamine (581 μL, 4.9 mmol) are added. The reaction stirred at room temperature 2 h. The reaction is partitioned between ethyl acetate and water. The organic layer is washed with saturated sodium bicarbonate, and saturated sodium chloride, dried (sodium sulfate), filtered, and concentrated under reduced pressure. Purification by flash column chromatography (silica, 40% ethyl acetate/hexane) provides the title compound. ESI MS m/z 376.1 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07176242B2 |
| 출처 데이터셋 | uspto-grants-2007_02 |
| ORD ID | ord-8a500f39426944db86cb3eecd30559c4 |
| 출처 메모 | uspto-grants-2007_02 |