HRID2383975
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 mixture of 50% NaH (4.6 g, 0.097 mol) in dimethoxymethane (20 ml) at room temperature under nitrogen was added drop wise at room temperature and under nitrogen a solution of 4-cyano-4-(4-methoxy-dibenzofuran-1-yl)-heptane dioic acid dimethyl ester (13.3 g, 0.032 mol) in dimethoxymethane (130 ml). The reaction mass was allowed to stir for 3 hrs at room temperature. Once product is formed, the reaction mass was quenched with water and extracted with ethyl acetate. The organic layer was dried with sodium sulfate and concentrated under vacuum. 5-cyano-5-(4-methoxy-dibenzofuran-1-yl)-2-oxo-cyclohexane carboxylic acid methyl ester was isolated by column chromatography. Yield 9.8 g (80%)
WORKUP
后处理
- additionwas added drop wise at room temperature
- customOnce product is formed
- customthe reaction mass was quenched with water
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried with sodium sulfate
- concentrationconcentrated under vacuum