HRID1533908

反应详情

EQUATION

反应方程式

HRID 1533908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.5 g (0.025 mol) of 1-(4-fluorophenyl)piperazine, 4.1 g (0.025 mol) of 5-(2-chloroethyl)-3-methyl-2-oxazolidinone, 8.0 g (0.075 mol) of anhydrous sodium carbonate and 0.4 g of potassium iodide in 150 mL of n-butanol was heated at reflux for 20 h. The mixture was concentrated under reduced pressure and the residue partitioned between water and benzene. The benzene layer was washed with water and brine, dried (Na2SO4) and concentrated under reduced pressure to obtain a solid which was recrystallized from 2-propanol isopropyl/ether to obtain 5.7 g (74%) of white solid, mp 82°-84° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 20 h
  3. concentrationThe mixture was concentrated under reduced pressure
  4. customthe residue partitioned between water and benzene
  5. washThe benzene layer was washed with water and brine
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated under reduced pressure
  8. customto obtain a solid which
  9. customwas recrystallized from 2-propanol isopropyl/ether