HRID2383975

反应详情

EQUATION

反应方程式

HRID 2383975 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added drop wise at room temperature
  2. customOnce product is formed
  3. customthe reaction mass was quenched with water
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic layer was dried with sodium sulfate
  6. concentrationconcentrated under vacuum