Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Methylmorpholine → 2-Amino-5-nitrobenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | 2-Amino-5-nitrobenzoic acid | HCID 12032 | — |
| 반응물 | Ammonium Hydroxide | HCID 14923 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Amino-5-nitrobenzamide | HCID 97665 | — |
반응 단계
To a mixture of 2-amino-5-nitro-benzoic acid (12.9 g, 81.9 mmol), 1-ethyl-3-(3′-dimethylaminopropyl)carbodiimide hydrochloride (EDCl) (17.3 g, 90.1 mmol), 1-hydroxybenzotriazole hydrate (HOBt) (12.2 g, 90.1 mmol) in THF (200 mL) was added 4-methylmorpholine (NMM) (9.91 mL, 90.1 mmol). After 10 minutes, ammonium hydroxide (50% v/v, 50 mL) was added. The mixture was stirred at room temperature under nitrogen for 17 hours. Solvent was removed under reduced pressure. Water was added. The solid separated was filtered, washed with aqueous NaHCO3 solution, and with water, and dried in air, to afford 2-amino-5-nitro-benzamide as a yellow solid. Yield: 9.88 g (66%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09238640B2 |
| 출처 데이터셋 | uspto-grants-2016_01 |
| ORD ID | ord-72088be0d9ba48f893e3b4b9895d13f0 |
| 출처 메모 | uspto-grants-2016_01 |