HRID1951665
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
PROCEDURE
实验过程
To a solution of 1.10 g (2.37 mmol) N-[6-chloro-4-(2-chloro-phenyl)-pyridin-3-yl]-2-(3-chloro-5-methoxy-phenyl)-N-methyl-isobutyramide in 20 ml CH2Cl2 4.74 ml (4.74 mmol) BBr3 (1 M in CH2Cl2) was added at 0° C. The reaction mixture was allowed to reach ambient temperature and stirred for 6 h After addition of 50 ml water the mixture was extracted three times with 60 ml CH2Cl2. The combined organic solvents were dried (Na2SO4), filtered and evaporated. The residue was purified by flash-chromatography (SiO2, CH2Cl2/ethyl acetate 4:1) to give 0.70 g (65%) of the title compound as a white foam. MS m/e (%): 449.1 (M+H+, 100).
WORKUP
后处理
- customto reach ambient temperature
- extractionwas extracted three times with 60 ml CH2Cl2
- dry with materialThe combined organic solvents were dried (Na2SO4)
- filtrationfiltered
- customevaporated
- customThe residue was purified by flash-chromatography (SiO2, CH2Cl2/ethyl acetate 4:1)