HRID1197513

反应详情

EQUATION

反应方程式

HRID 1197513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.08 g (3.3 mM) of 1-[2-(bis-(4-fluorophenyl)-methoxy)ethyl]piperazine and 0.97 g of 3-phenyl-5-chloromethyl-1,2,4-oxadiazole (prepared according to Chem.Ber. 105 (1972)2825) were dissolved in 5 ml of dry dimethylformamide. 1.4 g of potassium carbonate were added and the mixture was stirred at room temperature overnight. Toluene and water were added, the aqueous phase extracted with toluene, the combined organic phases washed three times with water, treated with charcoal and evaporated in vacuo. The residue was dissolved in 10 ml of ethanol and 0.69 g of maleic acid were added. The precipitate was isolated by filtration and recrystallized from hot acetonitrile to obtain the dimaleate salt of the title compound as colourless crystals melting at 142°-143°. Analytical data were in accordance with the proposed structure.

WORKUP

后处理

  1. extractionthe aqueous phase extracted with toluene
  2. washthe combined organic phases washed three times with water
  3. additiontreated with charcoal
  4. customevaporated in vacuo
  5. dissolutionThe residue was dissolved in 10 ml of ethanol
  6. addition0.69 g of maleic acid were added
  7. customThe precipitate was isolated by filtration
  8. customrecrystallized from hot acetonitrile