HRID654097

反应详情

EQUATION

反应方程式

HRID 654097 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(3-Chloropropyl)-4-(4-fluorophenyl)piperazine can be obtained as follows: a solution of 1-bromo-3-chloropropane (68 cc) and 4-(4-fluorophenyl)piperazine (50 g) in acetonitrile (400 cc) is stirred at 25° C. for 20 hours with potassium carbonate (97 g). The mixture is filtered and then concentrated to dryness under reduced pressure (2.7 kPa). The residue is chromatographed on a column of silica gel (0.2-0.063-mm particle size, 9-cm diameter, 60-cm height) and eluted with ethyl acetate, 500-cc fractions being collected. Fractions 5 to 7 are combined and concentrated to dryness under reduced pressure (2.7 kPa) to give 1-(3-chloropropyl)-4-(4-fluorophenyl)piperazine (44.4 g) in the form of a yellow oil.

WORKUP

后处理

  1. filtrationThe mixture is filtered
  2. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
  3. customThe residue is chromatographed on a column of silica gel (0.2-0.063-mm particle size, 9-cm diameter, 60-cm height)
  4. washeluted with ethyl acetate, 500-cc fractions
  5. custombeing collected
  6. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)