HRID80917

反应详情

EQUATION

反应方程式

HRID 80917 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 2,5-dibromo-4-methyl-pyridine (5.0 g, 20 mmol) and isopropyl-piperazine (25.6 g, 200 mmol) were added pyridine (2.06 g, 206 mmol). The reaction mixture was refluxed for 5 h under a nitrogen atmosphere. Brine was added and the mixture was extracted with EtOAc. The organic extract was washed with brine and 0.5 N hydrochloric acid. The acidic layer was made alkaline with Na2CO3 to pH 8 and then extracted with CH2Cl2. The organic extract was dried (Na2SO4) and concentrated to give 5.4 g (90%) of 1-(5-bromo-4-methyl-pyridin-2-yl)-4-isopropyl-piperazine.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 5 h under a nitrogen atmosphere
  2. extractionthe mixture was extracted with EtOAc
  3. extractionThe organic extract
  4. washwas washed with brine and 0.5 N hydrochloric acid
  5. extractionextracted with CH2Cl2
  6. extractionThe organic extract
  7. dry with materialwas dried (Na2SO4)
  8. concentrationconcentrated