HRID455143
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
A mixture of 2-(2-(4-chlorophenyl)imidazo[1,2-a]pyridin-3-yl)acetohydrazide (0.55 mmol, 1.0 eq) in DMF (1-2 ml) and picolinimidamide hydrochloride (1.5 eq) was heated at 120° C. for 3 h. The mixture was cooled to rt, treated with sat. NaHCO3 (5 ml), extracted with CH2Cl2 (10 ml). The organic solution was dried with Na2SO4, evaporated under vacuum. The crude product was purified by HPLC. M/e+ 387 for C21H16ClN6 (M+H)+; 1H-NMR (400 MHz, CD3OD) δ 9.11 (d, J=1.4 Hz, 1H), 8.56 (d, J=3.7 Hz, 1H), 8.36 (d, J=6.2 Hz, 2H), 7.77 (d, J=8.4 Hz, 2H), 7.70 (dt, J=8.4, 2.9 Hz, 2H), 7.36 (m, 2H), 6.99 (m, 2H), 4.64 (s, 2H) ppm.
WORKUP
后处理
- temperatureThe mixture was cooled to rt
- extractionextracted with CH2Cl2 (10 ml)
- dry with materialThe organic solution was dried with Na2SO4
- customevaporated under vacuum
- customThe crude product was purified by HPLC