Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylamine → N,N,3-trimethyl-4-nitrobenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylamine | HCID 674 | — |
| 반응물 | 3-Methyl-4-nitrobenzoic acid | HCID 18370 | — |
| 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 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N,N,3-trimethyl-4-nitrobenzamide | HCID 786992 | 73.17% |
반응 단계
To a solution of 3-methyl-4-nitrobenzoic acid (0.5 g, 2.76 mmol) in DMF (5 mL) was added DIPEA (1.06 g, 8.28 mmol), followed by HATU (1.57 g, 4.14 mmol) and dimethylamine (0.24 g, 5.52 mmol). The reaction mixture was stirred at room temperature for 12 h. The reaction mixture was then diluted with water and extracted with EtOAc. The organic layer was washed with brine, then concentrated to provide crude material which was further purified by column chromatography (silica:100-200 mesh, MeOH:DCM 8-10%), to afford the title compound (0.42 g, 73.17%). LCMS (ES+) 209 (M+H)+, RT 1.92 minutes (method 3).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09096614B2 |
| 출처 데이터셋 | uspto-grants-2015_08 |
| ORD ID | ord-15264fb989334572a52b0318e5672d67 |
| 출처 메모 | uspto-grants-2015_08 |