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
- -20 °C
PROCEDURE
实验过程
Methyl (2R,6S)-6-(4-chlorophenyl)piperidine-2-carboxylate (2.47 g) was added to a suspension of lithium aluminum hydride (508 mg) in THF (50 mL) in a nitrogen atmosphere at −20° C., and the reaction solution was stirred at −20° C. for one hour. Water (0.51 mL), a 5 N sodium hydroxide solution (0.51 mL), and water (1.53 mL) were sequentially added to the reaction solution at −20° C., and the reaction solution was stirred at room temperature for 15 minutes. Ethyl acetate was added to the reaction solution. Then, the reaction solution was filtered through celite, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (carrier: Chromatorex NH; elution solvent: heptane-ethyl acetate system) to obtain 1.90 g of the title compound. The property value of the compound is as follows.
WORKUP
后处理
- stirringthe reaction solution was stirred at room temperature for 15 minutes
- filtrationThen, the reaction solution was filtered through celite
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (carrier: Chromatorex NH; elution solvent: heptane-ethyl acetate system)