HRID1056649
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
A mixture of tert-butyl 9-((2-chloro-5-methylpyrimidin-4-yl)amino)-3-azaspiro[5.5]undecane-3-carboxylate (1.2 g, 3.0 mmol), 2,3-dimethylindazol-6-amine hydrochloride (896.5 mg, 4.536 mmol), diacetoxypalladium (132.4 mg, 0.5898 mmol), BINAP (370.3 mg, 0.5947 mmol) and dicesium carbonate (2.98 g, 9.15 mmol) was dissolved in anhydrous dioxane (10 mL). The reaction mixture was stirred under microwave irradiation at 150° C. for 2 h and then concentrated in vacuo. The residue was purified by silica gel column chromatography (DCM/MeOH (v/v)=30/1) to give the title compound as a yellow solid (1.04 g, 66%).
WORKUP
后处理
- concentrationconcentrated in vacuo
- customThe residue was purified by silica gel column chromatography (DCM/MeOH (v/v)=30/1)