反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 180 °C
PROCEDURE
实验过程
The title compound was prepared using 6-(6-chloro-imidazo[1,2-b]pyridazin-3-ylmethyl)-7-fluoro-quinoline (Intermediate J, 50 mg, 0.160 mmol), piperazin-2-one (80 mg, 0.799 mmol) and KF (27.9 mg, 0.480 mmol) were suspended in NMP (1.0 mL). The RM was stirred at 180° C. for 5 h. The mixture was diluted with EtOAc and washed with 1M NaHCO3 (1×) and water (2×). The combined organic layers were dried over Na2SO4, filtered and concentrated. The residue was purified by flash chromatography and afforded the title compound as a foam (tR 2.88 min (conditions 5), MH+=377, 1H-NMR in DMSO-d6: 8.85 (d, 1H); 8.33 (d, 1H); 8.07 (s, 1H); 7.98 (d, 1H); 7.83 (d, 1H); 7.74 (m, 1H); 7.5 (s, 2H); 7.11 (d, 1H); 4.41 (s, 2H); 4.00 (s, 2H); 3.67 (m, 2H); 3.26 (m, 2H)).
WORKUP
后处理
- customThe title compound was prepared
- washwashed with 1M NaHCO3 (1×) and water (2×)
- dry with materialThe combined organic layers were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by flash chromatography