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
- 130 °C
PROCEDURE
实验过程
A solution of 8-(1-ethyl-propyl)-3-iodo-2,6-dimethyl-imidazo[1,2-b]pyridazine (0.30 g, 0.87 mmol), 7-isopropyl-1,2-dimethyl-1H-indole (0.33 g, 1.76 mmol), Cs2CO3 (0.57 g, 1.75 mmol), and DMF (5 mL), is degassed with N2 for 20 minutes. Pd2(dba)3 (0.040 g, 0.044 mmol is added and the solution is heated at 130° C. overnight. The solution is diluted EtOAc (30 mL) washed with water (2×30 mL), brine (30 mL) dried over MgSO4, filtered and concentrated. The residue is purified by ISCO (20%-30% EtOAc gradient) to furnish the title compound (0.017 g, 0.042 mmol, 4.8%). 1H NMR (CDCl3), δ 1.14-1.46 (m, 6H), 1.76-1.95 (m, 4H), 2.30 (s, 3H), 2.42 (s, 3H), 2.45 (s, 3H), 3.38-3.48 (m, 1H), 3.86-3.97 (m, 1H), 4.04 (s, 3H), 6.64 (s, 1H), 6.99-7. LC/MS (m/z): calcd. for C26H34N4 (M+H)+: 403.3. found: 403.4.
WORKUP
后处理
- washwashed with water (2×30 mL), brine (30 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue is purified by ISCO (20%-30% EtOAc gradient)