HRID85157

反应详情

EQUATION

反应方程式

HRID 85157 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 benzyl 4-((6-(tert-butoxycarbonylamino)pyridin-3-yl)methyl)piperazine-1-carboxylate (104; 2.20 g, 5.20 mmol) in dichloromethane (10 mL) was added TFA (3.4 g, 31.2 mmol) at room temperature. The resulting reaction mixture was stirred at room temperature for 12 h and then concentrated under reduced pressure. Enough saturated aqueous Na2CO3 was added to adjust the pH=9. The resulting mixture was then extracted with dichloromethane (3×25 mL). The combined organic layers were dried (MgSO4) and concentrated under reduced pressure to afford benzyl 4-((6-aminopyridin-3-yl)methyl)piperazine-1-carboxylate 105 (1.50 g, 89%).

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. concentrationconcentrated under reduced pressure
  3. additionEnough saturated aqueous Na2CO3 was added
  4. extractionThe resulting mixture was then extracted with dichloromethane (3×25 mL)
  5. dry with materialThe combined organic layers were dried (MgSO4)
  6. concentrationconcentrated under reduced pressure