HRID2190333

反应详情

EQUATION

反应方程式

HRID 2190333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

3-bromo-1,1-diphenylpropane (2.6 g, 9 mmol) and tert-butyl 4-(2-aminoethyl)piperidine-1-carboxylate (4.7 g, 21 mmol) were mixed together in acetonitrile (100 ml) and potassium carbonate (1.3 g, 9 mmol) was added. The resulting mixture was heated to 65° C. with stirring under N2 overnight. After that time the mixture was cooled and concentrated under reduced pressure. The residue was partitioned between DCM and water. The DCM layer was washed with water, dried over MgSO4 and concentrated under reduced pressure to give the crude product as a clear oil. The crude product was purified by combiflash (0-10% MeOH/DCM) to give tert-butyl 4-(2-(3,3-diphenylpropylamino)ethyl)piperidine-1-carboxylate 48.

WORKUP

后处理

  1. temperatureAfter that time the mixture was cooled
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was partitioned between DCM and water
  4. washThe DCM layer was washed with water
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under reduced pressure
  7. customto give the crude product as a clear oil
  8. customThe crude product was purified by combiflash (0-10% MeOH/DCM)