Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dichloroethane → 3-bromo-4-(hydroxymethyl)-N-(3-(trifluoromethyl)phenyl)benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | 3-(Trifluoromethyl)aniline | HCID 7375 | — |
| 반응물 | HOAt | HCID 181649 | — |
| 반응물 | 3-Bromo-4-(hydroxymethyl)benzoic acid | HCID 19688415 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-bromo-4-(hydroxymethyl)-N-(3-(trifluoromethyl)phenyl)benzamide | HCID 90407963 | 35% |
반응 단계
EDC (1.3 equiv.) was added to a solution of 3-bromo-4-(hydroxymethyl)benzoic acid (1.0 equiv), 3-(trifluoromethyl)aniline (1.1 equiv.), HOAt (1.3 equiv.) in DMF (0.43 M). The mixture was stirred at ambient temperature 3 hrs. The reaction mixture was diluted with water and extracted with ethyl acetate. The combined extracts were washed sequentially with 1M aqueous sodium hydroxide and brine, dried over sodium sulfate, filtered, and concentrated. The residue was purified by ISCO(50% EtOAc/Heptane) to yield 3-bromo-4-(hydroxymethyl)-N-(3-(trifluoromethyl)phenyl)benzamide in 35% yield. LC/MS (m/z)=374.0 (MH+), Rt=0.93 min.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09242969B2 |
| 출처 데이터셋 | uspto-grants-2016_01 |
| ORD ID | ord-97272b5ef77b4a53bcffe989e86abaa7 |
| 출처 메모 | uspto-grants-2016_01 |