HRID85160
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of tert-butyl 5-(morpholinomethyl)pyridin-2-ylcarbamate (107; 1.40 g, 4.77 mmol) in dichloromethane (10 mL) was added TFA (10.0 mL). The mixture was stirred at room temperature for 12 h. The reaction mixture was concentrated under reduced pressure. Enough saturated aqueous Na2CO3 was added to the resulting residue to adjust the pH=9. The mixture was extracted with dichloromethane (3×25 mL). The combined organic layers were dried (MgSO4) and concentrated under reduced pressure to afford 5-(morpholinomethyl)pyridin-2-amine 108 (0.85 g, 92%).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- additionEnough saturated aqueous Na2CO3 was added to the resulting residue
- extractionThe mixture was extracted with dichloromethane (3×25 mL)
- dry with materialThe combined organic layers were dried (MgSO4)
- concentrationconcentrated under reduced pressure