HRID279298
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
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
1-(4-Chlorobenzyl)-4-[{(N-Boc-valyl)amino}methyl]piperidine (1.1 g, 2.51 mmol) was dissolved in 3 M HCl-CH3OH solution (25 mL) and stirred at 25° C. for 1 h. The reaction mixture was concentrated and the resulting salt was dissolved in 3:1 tBuOH-H2O (25 mL). Anion (OH−) exchange resin was added until the solution was slightly basic. Filtration and concentration afforded 1-(4-chlorobenzyl)-4-{(valylamino)methyl}piperidine (819 mg, 97%) which required no further purification: RPLC (97%); ESI/MS 338.1 (M++H, C18H28ClN3O).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- dissolutionthe resulting salt was dissolved in 3:1 tBuOH-H2O (25 mL)
- additionAnion (OH−) exchange resin was added until the solution
- filtrationFiltration and concentration