HRID1478028
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
- 150 °C
PROCEDURE
实验过程
To a suspension of tert-butyl 9-((2-chloro-5-methylpyrimidin-4-yl)amino)-3-azaspiro[5.5]undecane-3-carboxylate (332.2 mg, 0.84 mmol) and 1-methyl-1H-pyrazol-4-amine hydrochloride (252.2 mg, 1.89 mmol) in n-BuOH (8 mL) was added DIPEA (445.9 mg, 3.45 mmol). The reaction mixture was stirred at 150° C. in a sealed tube for 16 h and concentrated in vacuo. The residue was purified by silica gel column chromatography (MeOH/DCM (v/v)=1/20) to give the title compound as yellow oil (0.38 g, 99%).
WORKUP
后处理
- concentrationconcentrated in vacuo
- customThe residue was purified by silica gel column chromatography (MeOH/DCM (v/v)=1/20)