HRID370519

反应详情

EQUATION

反应方程式

HRID 370519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,3-Lutidine (321 g) was added with stirring to a solution of sodamide (351 g) in liquid ammonia (3 1). 1-Amino-3-chloropropane hydrochloride (429g) was added to this mixture over 8 minutes with stirring. Any liquid ammonia lost through evaporation was replaced. After 2 hours the reaction was quenched by the addition of ammonium chloride (120 g) and the reaction mixture was left to stand overnight to allow substantially complete escape of ammonia through evaporation. The residue so obtained was diluted with water (2 1) and extracted with dichloromethane. The extracts were dried (Na2SO4), the dichloromethane removed by evaporation and the residue distilled in vacuo to give 4-(3-methyl-2-pyridyl) butylamine (306.6 g).

WORKUP

后处理

  1. customAny liquid ammonia lost through evaporation
  2. customAfter 2 hours the reaction was quenched by the addition of ammonium chloride (120 g)
  3. waitthe reaction mixture was left
  4. customthrough evaporation
  5. customThe residue so obtained
  6. extractionextracted with dichloromethane
  7. dry with materialThe extracts were dried (Na2SO4)
  8. customthe dichloromethane removed by evaporation
  9. distillationthe residue distilled in vacuo