HRID1725764

反应详情

EQUATION

反应方程式

HRID 1725764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 4-acetylpyridine (75 mL, 0.68 mol) and ethyl formate (109 mL) in anhydrous benzene (1 L) was added sodium methoxide (73 g) and the resulting mixture was refluxed for 18 hours. The mixture was cooled and benzene decanted from a sticky solid, which had formed during the reaction. The crude product was dissolved in water (700 mL) and hydrazine dihydrochloride was added and the resulting mixture was stirred at room temperature for 2 hours. The mixture was redissolved by addition of 5N NaOH. Precipitate formed which was removed by filtration and dried to give 4-(1H-pyrazol-3-yl)pyridine (35 g).

WORKUP

后处理

  1. temperaturethe resulting mixture was refluxed for 18 hours
  2. temperatureThe mixture was cooled
  3. custombenzene decanted from a sticky solid
  4. customwhich had formed during the reaction
  5. customPrecipitate formed which
  6. customwas removed by filtration
  7. customdried