Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Nitroformic Acid → 4-Nitrobenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Nitroformic Acid | HCID 88689 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-Nitrobenzamide | HCID 12091 | — |
반응 단계
A mixture of nitrocarboxylic acid (NB-2 or NB-3; 1.2 equivalents), amine (A13, A14 or A16; 1.1 equivalents), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.2 equivalents), and 1-hydroxybenzotriazole hydrate (1.2 equivalents) in DMF (0.79 M) was stirred at room temperature for 4 hours. The mixture was diluted with dichloromethane (100 mL) and washed with aqueous saturated sodium bicarbonate solution (50 mL). The aqueous layer was re-extracted with dichloromethane (2×50 mL) and the combined organic solution was dried (Na2SO4), filtered and evaporated under reduced pressure. The crude mixture was purified on silica gel column to provide the 4-nitrobenzamide (NB-2-A13, NB-2-A14 or NB-3-A16).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07749530B2 |
| 출처 데이터셋 | uspto-grants-2010_07 |
| ORD ID | ord-d8a31030a5384adb8d45fd76dc799c9c |
| 출처 메모 | uspto-grants-2010_07 |