HRID970398

反应详情

EQUATION

反应方程式

HRID 970398 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

N-(t-butoxycarbonyl)-4-(4-fluorophenylmethyl)piperidine (11.2 g, 38.2 mmol) was dissolved in 4M HCl in dioxane (50 mL). The reaction was stirred for 15 min and then conc. in vacuo to a white solid. The solid was dissolved in 3% MeOH/CH2Cl2 in EtOAc/MeOH while warming once all solids were dissolved hexanes was added. The crystallization was allowed to cool to room temperature and then placed at 4° C. for 16 h. The white solids were filtered off to yield 8.4 g of product. MS (ESI) 194 (M−HCl+H).

WORKUP

后处理

  1. temperaturewhile warming once all solids
  2. additionwas added
  3. customThe crystallization
  4. waitplaced at 4° C. for 16 h
  5. filtrationThe white solids were filtered off