Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2,4-Benzenetriamine, hydrochloride (1:2) → 2,3-Bis(4-hydroxyphenyl)quinoxalin-6-ylamine Dihydrochloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2,4-Benzenetriamine, hydrochloride (1:2) | HCID 94179 | — |
| 반응물 | 4,4'-Dihydroxybenzil | HCID 458204 | — |
| 용매 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 생성물 | 2,3-Bis(4-hydroxyphenyl)quinoxalin-6-ylamine Dihydrochloride | HCID 135610078 | 167.3% |
반응 단계
98.04 mg (0.5 mmol) of 1,2,4-benzenetriamine dihydrochloride and 121.2 mg (0.5 mmol) of 4,4′-dihydroxybenzil were dissolved in 2 ml of 1:1 mixture of dioxane-water. The reaction was refluxed for 3 hours. Then solvent was removed in vacuo. The residue was dissolved in 2 ml of methanol and this solution was added dropwise to 40 ml of diethyl ether. The formed dark-red precipitate was collected, washed with ether and dried in vacuo to give 168.3 mg (83.7% yield) of the product. 98.7% purity by LC/MS (230 DAD). Mass-spec [ES+]=330.8. 1H NMR (500 MHz, MeOH-d4) 6.76–6.77 (2H, d), 6.87–6.89 (2H, d), 7.05–7.06 (1H, d), 7.29–7.31 (2H, d), 7.38–7.40 (2H, d), 7.50–7.52 (1H, m), 7.99–8.01 (1H, d).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07208493B2 |
| 출처 데이터셋 | uspto-grants-2007_04 |
| ORD ID | ord-930be883949d4e908b6e89054035383d |
| 출처 메모 | uspto-grants-2007_04 |