HRID279281
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 3-[{N-(tert-butoxycarbonyl)glycyl}aminomethyl]-1-(4-chlorobenzyl)pyrrolidine (804 mg, 2.11 mmol) in methanol (10 mL) was added 4 N HCl in dioxane (5 mL). The solution was stirred at room temperature for 3.5 h. The reaction mixture was concentrated and 1 N NaOH solution (20 mL) was added. The mixture was extracted with dichloromethane (20 mL×3), and the combined extracts were dried over sodium sulfate and concentrated to give desired 1-(4-chlorobenzyl)-3-{(glycylamino)methyl)pyrrolidine (599 mg, 100%): The purity was determined by RPLC/MS (100%); ESI/MS m/e 282.2 (M++H, C14H20ClN3O).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- addition1 N NaOH solution (20 mL) was added
- extractionThe mixture was extracted with dichloromethane (20 mL×3)
- dry with materialthe combined extracts were dried over sodium sulfate
- concentrationconcentrated