HRID1275231
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 mixture of 4-hydroxy-4-phenylpiperidine (5 g, 0.0282 mol), N-benzyloxycarbonyl-3-bromopropylamine (8.445 g, 0.031 mol), and potassium carbonate (7.795 g, 0.0564 mole) in acetone (200 mL) was stirred and refluxed for 12 hours. Acetone was evaporated at reduced pressure, the residue was treated with ice-cold water (400 mL) and extracted with CH2Cl2 (4×120 mL). Solvent was evaporated from the combined dried (sodium sulfate) extracts and the residue was found to be almost pure desired product (9.5 g, 91%) by tlc and 1H-NMR and was used as such without any further purification.
WORKUP
后处理
- temperaturerefluxed for 12 hours
- customAcetone was evaporated at reduced pressure
- additionthe residue was treated with ice-cold water (400 mL)
- extractionextracted with CH2Cl2 (4×120 mL)
- customSolvent was evaporated from the
- dry with materialcombined dried (sodium sulfate) extracts
- customsuch without any further purification