HRID1432573
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
PROCEDURE
实验过程
To a solution of 8-(1-Ethyl-propyl)-2,6-dimethyl-3-(3-methyl-thiophen-2-yl)-imidazo[1,2-b]pyridazine (8.83 g, 28.17 mmol) and CH2Cl2 (90 mL) is added NBS (5.26 g, 29.58 mmol). The solution is stirred at ambient temperature for 2 hours. The solution is washed with water (3×75 mL), dried over MgSO4, filtered and concentrated to furnish the title compound (10.5 g, 26.76 mmol, 95%). 1H NMR (CDCl3), δ 0.87 (t, J=7.3 Hz, 6H), 1.73-1.93 (m, 4H), 2.09 (s, 3H), 2.44 (s, 3H), 2.51 (s, 3H), 3.26-3.36 (m, 1H), 6.68 (s, 1H), 6.98 (d, J=4.9 Hz, 1H) ppm. LC/MS (m/z): calcd. for C18H22BrN3S (M+H)+: 392.6; found: 392.1, 394.1.
WORKUP
后处理
- washThe solution is washed with water (3×75 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated