Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Hydroxide → 3-[3-(5-Bromo-3-methylpyrid-2-yl)propyl]-6-(3-pyridylmethyl)-3H-1,2,3-triazolo[5,4-b]pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 2-[3-(5-Bromo-3-methylpyrid-2-yl)-propylamino]-3-amino-5-(pyrid-3-ylmethyl)pyridine | HCID 19851776 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 용매 | Sulfuric Acid | HCID 1118 | — |
| 생성물 | 3-[3-(5-Bromo-3-methylpyrid-2-yl)propyl]-6-(3-pyridylmethyl)-3H-1,2,3-triazolo[5,4-b]pyridine | HCID 19851790 | 57% |
반응 단계
Sodium nitrite solution (1.02 g in 50 ml water) was added dropwise over 25 minutes to a stirred and cooled solution of 2-[3-(5-bromo-3-methylpyrid-2-yl)-propylamino]-3-amino-5-(pyrid-3-ylmethyl)pyridine (4.7 g) in sulphuric acid (molar, 200 ml) keeping the temperature at 4° C. Reaction was stirred at 4° C. for a further hour and was then left in the fridge overnight and then warmed to room temperature. The reaction mixture was basified to pH 13 with sodium hydroxide solution (10 M). Chloroform extraction of the reaction mixture gave the crude product which was then chromatographed on silica in methanol/chloroform 1:19 and then recrystallised from acetonitrile to give the title compound (2.75 g), m.p. 109°-110° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04863933 |
| 출처 데이터셋 | uspto-grants-1989_09 |
| ORD ID | ord-235d2c5d355c42e8930c9cc34fd311f8 |
| 출처 메모 | uspto-grants-1989_09 |