Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → 3,5-Dimethyl-3H-[1,2,3]triazolo[4,5-b]pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Tert-Butyl nitrite | HCID 10906 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | N2,6-Dimethylpyridine-2,3-diamine | HCID 22036951 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3,5-Dimethyl-3H-[1,2,3]triazolo[4,5-b]pyridine | HCID 45079445 | 76.2% |
반응 단계
6,N2-dimethyl-pyridine-2,3-diamine of Step A (1.5 g, 10.9 mmol), 2-methyl-2-nitrosooxy-propane (1.6 ml, 13.1 mmol), acetic acid (2.6 ml, 43.6 mmol), and ethanol (50 ml) were stirred at 60° C. for 60 min. After cooling to ambient temperature, sodium hydrogen carbonate (3 g) was added and the resulting mixture was stirred at ambient temperature for 20 min. The mixture was diluted with dichloromethane (20 ml), solids were filtered off, and the obtained solution was concentrated in vacuum. Chromatography on silica gel, eluting with dichloromethane-acetonitrile (93:7) yielded the title compound (1.23 g, 76%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07417041B2 |
| 출처 데이터셋 | uspto-grants-2008_08 |
| ORD ID | ord-e3448136d0034f319c88efeaf03f69a2 |
| 출처 메모 | uspto-grants-2008_08 |