HRID1734122
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 0.4 g (2.9 mmol) of 3-amino-2-methoxy-4-methylpyridine and 0.5 g (2.9 mmol) of 2-chloronicotinoyl chloride in EtOAc at 0° C. was added 0.4 g (3.0 mmol) of N,N-diisopropylethylamine. Stirring was continued for 10 h at which point the mixture was washed with 0.1N HCl , dried (MgSO4), concentrated and purified by flash chromatography on silica gel (1:1 EtOAc:hexanes) to yield 0.7 g (88%) of the desired material. m.p.: 145°-146° C. (Recrystallized from ethyl acetate).
WORKUP
后处理
- washthe mixture was washed with 0.1N HCl
- dry with materialdried (MgSO4)
- concentrationconcentrated
- custompurified by flash chromatography on silica gel (1:1 EtOAc:hexanes)