反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 8.0 g. (0.0343 mole) of 1-(3-chlorophenyl)piperazine hydrocloride, 5.88 g. (0.0343 mole) of 1-bromo-4-chlorobutane, 9.48 g. (0.9686 mole) of finely powdered potassium carbonate, and 200 ml. of dry xylene was refluxed for 22 hr. To this mixture there was then added 5.39 g. (0.0343 mole) of sodium 1,2,4-triazolo[4,3-a]pyridin-3(2H)-one, and the resulting suspension was refluxed an additional 72 hr. The mixture was then cooled, diluted with 200 ml. of chloroform, stirred for 15 min. and filtered. The clear filtrate was concentrated to an oil (9.8 g.) under reduced pressure. The residue was recrystallized from ET2O--EtOH--CHCl3 to afford 2.31 g. (43%) of the desired product, m.p. 122°-123°.
WORKUP
后处理
- additionA mixture of 8.0 g
- additionTo this mixture there was then added 5.39 g
- temperatureThe mixture was then cooled
- additiondiluted with 200 ml
- filtrationfiltered
- concentrationThe clear filtrate was concentrated to an oil (9.8 g.) under reduced pressure
- customThe residue was recrystallized from ET2O
- customEtOH--CHCl3 to afford 2.31 g