HRID597872

反应详情

EQUATION

反应方程式

HRID 597872 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a solution of 4-chloro iodobenzene (25 g) in 400 mL CH2Cl2 at room temperature was added propargyl amine (13.5 mL), diisopropyl amine (37 mL), CuI (4 g) and Pd(PPh3)2Cl2 (3.7 g). The mixture was stirred overnight at room temperature, diluted with 600 mL EtOAc and filtered through a CELITE pad to remove insoluble materials. The solution washed with water, brine, dried over MgSO4, concentrated and purified by chromatography to provide 14.1 g of 3-(4-chloro-phenyl)-prop-2-ynylamine. MS: m/e 166.1 (MH+)

WORKUP

后处理

  1. filtrationfiltered through a CELITE pad
  2. customto remove insoluble materials
  3. washThe solution washed with water, brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. custompurified by chromatography