HRID365452
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
Ethyl 1-(t-butoxycarbonyl)piperidine-3(S)-carboxylate (35.9 g, 0.099 mol) was dissolved in abs EtOH (70 mL), treated with 0.5N NaOH (418 mL, 0.209 mol), and heated at reflux for 0.75 h. The reaction mixture was cooled and extracted with EtOAc. The aqueous basic layer was cooled with ice, carefully acidified (pH 3) with 3N HCl and extracted with CH2Cl2 (3×100 mL). The organics were combined, dried (MgSO4), filtered, and concentrated to give the title compound.
WORKUP
后处理
- temperatureheated
- temperatureat reflux for 0.75 h
- temperatureThe reaction mixture was cooled
- extractionextracted with EtOAc
- temperatureThe aqueous basic layer was cooled with ice
- extractionextracted with CH2Cl2 (3×100 mL)
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated