Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzaldehyde → 7-Bromo-2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-5-ylamine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzaldehyde | HCID 240 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 4-Bromo-2,6-diaminopyridine | HCID 11435393 | — |
| 반응물 | O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine | HCID 11830845 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 7-Bromo-2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-5-ylamine | HCID 22629673 | 39.3% |
반응 단계
To a solution of 96 mg (0.51 mmol) 4-bromo-pyridine-2,6-diamine in 2.4 ml MeOH was added 121 mg (0.56 mmol) O-mesitylenesulfonylhydroxylamine (prepared from ethyl o-mesitylene-sulfonylacetohydroxamate and HClO4 (70%)) in 0.6 ml MeOH at −5° C. and after 15min 71 mg (0.56 mmol) benzaldehyde and stirred for 30 min. The addition of 4.8 ml 1N KOH was followed by extraction with ethylacetate, drying of the organic layer with Na2SO4, and removal of the volatile components. The residue was purified by column chromatography on silica eluting with ethylacetate and hexane (2:3). 58 mg(39%) of 7-bromo-2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-5-ylamine were isolated, MS m/e (%): 290 (M++2, 44).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06355653B1 |
| 출처 데이터셋 | uspto-grants-2002_03 |
| ORD ID | ord-b9ea05ca0bc7405d99a5acc2a36743a9 |
| 출처 메모 | uspto-grants-2002_03 |