HRID1437274

反应详情

EQUATION

反应方程式

HRID 1437274 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Diethyl oxalate (4.42 mL) was added to sodium ethoxide (2.22 g) in ethanol (22 mL), and the mixture was stirred for 10 minutes. The above-obtained 1-(4-methyl-2-pyridyl)ethanone (2.20 g) in ethanol (22 mL) was added to the mixture, followed by stirring at room temperature for 20 minutes. Water was added to the reaction mixture, and the resultant mixture was washed with diethyl ether, and then the aqueous layer was partitioned by use of saturated aqueous ammonium chloride and chloroform. The organic layer was dried over sodium sulfate anhydrate, followed by filtration. The solvent was removed under reduced pressure, to thereby give 4-(4-methyl-2-pyridyl)-2,4-dioxobutanoic acid ethyl ester as an oily product (2.84 g, 74%).

WORKUP

后处理

  1. stirringby stirring at room temperature for 20 minutes
  2. washthe resultant mixture was washed with diethyl ether
  3. customthe aqueous layer was partitioned by use of saturated aqueous ammonium chloride and chloroform
  4. dry with materialThe organic layer was dried over sodium sulfate anhydrate
  5. filtrationfollowed by filtration
  6. customThe solvent was removed under reduced pressure