HRID1275231

反应详情

EQUATION

反应方程式

HRID 1275231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturerefluxed for 12 hours
  2. customAcetone was evaporated at reduced pressure
  3. additionthe residue was treated with ice-cold water (400 mL)
  4. extractionextracted with CH2Cl2 (4×120 mL)
  5. customSolvent was evaporated from the
  6. dry with materialcombined dried (sodium sulfate) extracts
  7. customsuch without any further purification