HRID279298

反应详情

EQUATION

反应方程式

HRID 279298 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionthe resulting salt was dissolved in 3:1 tBuOH-H2O (25 mL)
  3. additionAnion (OH−) exchange resin was added until the solution
  4. filtrationFiltration and concentration