HRID394545
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
A solution of dry HCl.OEt2 was added to a solution of piperidine (7) (20.2 g, 54.36 mmol) in MeOH (200 mL) until pH˜1. The mixture was stirred at room temperature for 30 minutes. Solvent was evaporated, the residue was dissolved in CH2Cl2 (300 mL) and stirred with 1N NaOH (100 mL) for 15 minutes. The solvent was separated, washed with NaHCO3, and dried over MaSO4. The crude oil was purified by flash chromatography (CH2Cl2-MeOH(saturated with NH3)/95:5) to give a white solid (13.25 g, 84.6%).
WORKUP
后处理
- customSolvent was evaporated
- dissolutionthe residue was dissolved in CH2Cl2 (300 mL)
- stirringstirred with 1N NaOH (100 mL) for 15 minutes
- customThe solvent was separated
- washwashed with NaHCO3
- customdried over MaSO4
- customThe crude oil was purified by flash chromatography (CH2Cl2-MeOH(saturated with NH3)/95:5)