HRID2389912

反应详情

EQUATION

反应方程式

HRID 2389912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of dimethyl 5-(2-methoxy-2-oxoethoxy)-2-(3-methoxy-3-oxopropyl)pyridine-3,4-dicarboxylate (2.20 g, 5.96 mmol) in methanol (60 mL) was added sodium methoxide (0.805 g, 14.9 mmol) at 80° C., and the mixture was stirred for 30 min. The resulting precipitate was collected by filtration, washed with methanol, and dissolved in 1M hydrochloric acid (10 mL). The mixture was extracted with ethyl acetate and the extract was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by recrystallization (ethyl acetate/diisopropyl ether) to give the title compound (1.35 g, yield 67%).

WORKUP

后处理

  1. filtrationThe resulting precipitate was collected by filtration
  2. washwashed with methanol
  3. dissolutiondissolved in 1M hydrochloric acid (10 mL)
  4. extractionThe mixture was extracted with ethyl acetate
  5. dry with materialthe extract was dried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue was purified by recrystallization (ethyl acetate/diisopropyl ether)