HRID1518519

反应详情

EQUATION

反应方程式

HRID 1518519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 2-chloro-3-nitropyridine (5.0 g, 31.53 mmol) in anhydrous NMP (100 mL) was added tert-butylamine (10 mL, 94.52 mmol). The solution was heated at 60° C. for 14 hours and cooled. The mixture was poured into 1N HCl solution (400 mL) and extracted with EtOAc (3×150 mL). The combined organic layers were washed with saturated NaHCO3 solution and dried over MgSO4. After filtration, the solvent was evaporated under vacuum to afford N-tert-butyl-3-nitropyridin-2-amine as dark brown syrup.

WORKUP

后处理

  1. temperaturecooled
  2. extractionextracted with EtOAc (3×150 mL)
  3. washThe combined organic layers were washed with saturated NaHCO3 solution
  4. dry with materialdried over MgSO4
  5. filtrationAfter filtration
  6. customthe solvent was evaporated under vacuum