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
Anhydrous piperazine (5.6 g) was dissolved in methylene chloride (100 ml) to which was subsequently added triethylamine (4.5 ml). With cooling in an ice bath, to this was added dropwise 2-chlorobenzoxazole (3.7 ml) in small portions, followed by 45 minutes of stirring. The reaction solution was mixed with water, extracted with methylene chloride and then washed with saturated sodium bicarbonate aqueous solution and saturated brine in that order. The organic layer was dried with magnesium sulfate and the solvent was evaporated under a reduced pressure. Thereafter, the thus obtained mixture was purified by a silica gel column chromatography (methanol) to obtain the title compound 2-(1-piperazinyl)benzoxazole (4.751 g) in the form of yellow crystalline powder.
WORKUP
后处理
- temperatureWith cooling in an ice bath
- extractionextracted with methylene chloride
- washwashed with saturated sodium bicarbonate aqueous solution and saturated brine in that order
- dry with materialThe organic layer was dried with magnesium sulfate
- customthe solvent was evaporated under a reduced pressure
- customThereafter, the thus obtained mixture was purified by a silica gel column chromatography (methanol)