HRID1049236
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
- 65 °C
PROCEDURE
实验过程
A solution of N-(6-methyl-5-((2-(1-methyl-1H-pyrazol-4-yl)pyridin-4-yl)oxy)pyridin-2-yl)acetamide (3.88 g, 12.00 mmol) in THF (30 mL) was treated with 2M HCl (30 mL, 60 mmol), heated at 65° C. for 6 h, cooled to RT and concentrated to dryness. The mixture was treated with H2O, neutralized with solid NaHCO3, extracted with EtOAc (2×) and the combined organics were washed with brine, dried over Na2SO4 and concentrated to dryness. The material was suspended in 3:2 EtOAc/Hex, sonicated and the resulting solid collected via filtration and dried to afford 6-methyl-5-((2-(1-methyl-1H-pyrazol-4-yl)pyridin-4-yl)oxy)pyridin-2-amine (3.1 g, 92%) as a white solid. MS (ESI) m/z: 282.1 (M+H+).
WORKUP
后处理
- temperaturecooled to RT
- concentrationconcentrated to dryness
- additionThe mixture was treated with H2O
- extractionextracted with EtOAc (2×)
- washthe combined organics were washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated to dryness
- customsonicated
- filtrationthe resulting solid collected via filtration
- customdried