Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Hydroxybenzotriazole → 2-fluoro-5-nitro-N-(1,3-benzodioxol-5-ylmethyl)benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | Benzo-1,3-dioxole-5-methylamine | HCID 75799 | — |
| 반응물 | 2-Fluoro-5-nitrobenzoic acid | HCID 280997 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-fluoro-5-nitro-N-(1,3-benzodioxol-5-ylmethyl)benzamide | HCID 22467641 | 86.1% |
반응 단계
A mixture of 2-fluoro-5-nitrobenzoic acid (1.00 g), (1,3-benzodioxol-5-ylmethyl)amine (980 mg), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (1.55 g) and 1-hydroxybenzotriazole (1.09 g) in anhydrous dimethylformamide (10 mL) was stirred for 40 hours at ambient temperature. The mixture was partitioned between water and ethyl acetate. The separated organic layer was washed with an aqueous saturated sodium bicarbonate solution, 1N-hydrochloric acid, water and brine. Then, the resultant was dried over magnesium sulfate and evaporated in vacuo. The residue was triturated with diisopropyl ether to give 2-fluoro-5-nitro-N-(1,3-benzodioxol-5-ylmethyl)benzamide as yellow powders (1.48 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06384080B1 |
| 출처 데이터셋 | uspto-grants-2002_05 |
| ORD ID | ord-829a96a6ccff41a995f08c54de850f1f |
| 출처 메모 | uspto-grants-2002_05 |