HRID552385

反应详情

EQUATION

反应方程式

HRID 552385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-fluoronitrobenzene (5.00 g, 35.4 mmol) in THF (50 mL), 1-isopropylpiperazine (4.54 g, 35.4 mmol) and K2CO3 (7.35 g, 53.2 mmol) are added. The reaction mixture is stirred at room temperature overnight. The solvent is removed under reduced pressure and the residue is partitioned between EtOAc and water. The organic layer is washed with brine, dried (MgSO4), filtered and the solvent is removed under reduced pressure. The crude compound is purified by silica gel column chromatography using 99:1 and 98:2 DCM:NH3 (7 M in MeOH) to give the title compound (8.2 g, 94%).

WORKUP

后处理

  1. customThe solvent is removed under reduced pressure
  2. customthe residue is partitioned between EtOAc and water
  3. washThe organic layer is washed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent is removed under reduced pressure
  7. customThe crude compound is purified by silica gel column chromatography