Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 2-Amino-4-fluorobenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 4-Fluoroanthranilic acid | HCID 2724967 | — |
| 반응물 | Ammonia methanol | HCID 21705897 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Amino-4-fluorobenzamide | HCID 10241004 | 72.7% |
반응 단계
To solution of 2-amino-4-fluorobenzoic acid (4.0 g, 25.8 mmol) in degassed DMF (50 mL) were added HOBt (4.19 g, 31 mmol), DIEA (5.4 mL, 31 mmol), EDCI (5.94 g, 31 mmol) and 2N NH3/MeOH (18 mL, 36.1 mmol). The solution was stirred at rt for 48 h, and then concentrated under reduced pressure. The residue was purified by silica gel chromatography to afford 2-amino-4-fluorobenzamide as a solid (2.89 g, 66%). 1H NMR (300 MHz, DMSO-d6) δ 6.28 (m, 1H), 6.44 (m, 1H), 6.90 (br s, 2H), 7.08 (m, 1H), 7.58 (m, 1H), 7.71 (br d, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09308207B2 |
| 출처 데이터셋 | uspto-grants-2016_04 |
| ORD ID | ord-1a734152fcc34c9aafc56644849d0576 |
| 출처 메모 | uspto-grants-2016_04 |