HRID53528

反应详情

EQUATION

反应方程式

HRID 53528 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium methoxide (26.1 g) was added to a solution of 2-chloro-4-methyl-5-nitropyridine (19.0 g) in methanol (100 ml) and the resulting mixture was refluxed for 12 hours. Upon cooling, the mixture was poured over water (1 L), and the product was extracted with ethyl acetate and washed with water. The organic phase was dried (anhydrous magnesium sulfate) and concentrated, and the residue dissolved in hot ether and filtered. Crystallization from ether provided 10.2 g of the title compound, suitable for use in the next reaction.

WORKUP

后处理

  1. temperaturethe resulting mixture was refluxed for 12 hours
  2. temperatureUpon cooling
  3. extractionthe product was extracted with ethyl acetate
  4. washwashed with water
  5. dry with materialThe organic phase was dried (anhydrous magnesium sulfate)
  6. concentrationconcentrated
  7. dissolutionthe residue dissolved in hot ether
  8. filtrationfiltered
  9. customCrystallization from ether