反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
2-[4-[5-amino-6-(3-phenylisoxazol-5-yl)pyrazin-2-yl]-2-pyridyl]-2-methyl-propanenitrile (90 mg, 0.2353 mmol) was added to methanol (3 mL) followed by the addition of 1 M sodium hydroxide (705.9 μL of 1 M, 0.7059 mmol). The mixture was heated in the microwave for 90 minutes at 110° C. The reaction was cooled to ambient temperature and diluted with ethyl acetate/water. The organic layer was washed with brine (×1). The aqueous layer was acidified to pH3 with 1 M hydrochloric acid, extracted with ethyl acetate (×3) and the combined organic extracts washed with brine (×1). The extracted organic layer was dried over MgSO4, filtered and concentrated in vacuo to yield 2-[4-[5-amino-6-(3-phenylisoxazol-5-yl)pyrazin-2-yl]-2-pyridyl]-2-methyl-propanoic acid as white solid (40 mg, 42%) LC/MS m/z 401.1 [M+H]+.
WORKUP
后处理
- temperatureThe reaction was cooled to ambient temperature
- washThe organic layer was washed with brine (×1)
- extractionextracted with ethyl acetate (×3)
- washthe combined organic extracts washed with brine (×1)
- dry with materialThe extracted organic layer was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo