HRID1942064
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
- 180 °C
PROCEDURE
实验过程
(rac)-6-[1-(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-ethyl]-5,7-difluoro-quinoline (Intermediate C, 50 mg, 0.145 mmol), KF (84 mg, 1.45 mmol) and 1-methylpiperazine-2-one hydrochloride (65 mg, 0.435 mmol) were suspended in NMP (0.483 mL). The RM was stirred at 180° C. for 5 h. The mixture was filtered and the obtained filtrate was purified by reverse phase chromatography (water+0.1% TFA/acetonitrile+0.1% TFA). The collected fractions were concentrated and the residue was dissolved in MeOH, passed through an SPE cartridge of PL-HCO3 MP. The filtrate was concentrated to afford the title compound as a brownish oil (tR 3.19 min (conditions 1), MH+=423).
WORKUP
后处理
- filtrationThe mixture was filtered
- customthe obtained filtrate was purified by reverse phase chromatography (water+0.1% TFA/acetonitrile+0.1% TFA)
- concentrationThe collected fractions were concentrated
- dissolutionthe residue was dissolved in MeOH
- concentrationwas concentrated