HRID2169231
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
- 60 °C
PROCEDURE
实验过程
To a stirred solution of (3-phenyl-pyridin-2-yl)-acetonitrile (159) (4.9 g, 25.26 mmol) in ethanol (250 mL) was added 50% aqueous NH2OH (3.4 mL, 50.51 mmol) and the mixture was heated at 60° C. for 16 h. Silica thin layer chromatography was performed (40% ethyl acetate in hexane, Rf=0.2). Ethanol was evaporated, water (50 mL) was added, the mixture was extracted with etylacetate (3×50 mL), dried and concentrated to get N-hydroxy-2-(3-phenyl-pyridin-2-yl)-acetamidine (160) (5.3 g, 92.33%, crude) as a yellow solid.
WORKUP
后处理
- customEthanol was evaporated
- additionwater (50 mL) was added
- extractionthe mixture was extracted with etylacetate (3×50 mL)
- customdried
- concentrationconcentrated