HRID2359104

反应详情

EQUATION

反应方程式

HRID 2359104 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 4-bromo-2-aminopyridine (580 mmol) in 1.5 L dichloromethane was added pyridine (1.16 mol). The mixture was stirred for 20 min. Propionyl chloride (669 mmol) was added dropwise. The reaction mixture was stirred at room temperature for 5 h. Water was added and the reaction mixture was extracted with dichloromethane. The combined organic layer was washed with brine, dried and concentrated. The residue was recrystallized from hexane/ethyl acetate (6:1) to afford 112 g of N-(4-bromopyridin-2-yl)propanamide (85% yield).

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at room temperature for 5 h
  2. extractionthe reaction mixture was extracted with dichloromethane
  3. washThe combined organic layer was washed with brine
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was recrystallized from hexane/ethyl acetate (6:1)