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
5.0 Grams of 6-(1-oxo-2-chloroethyl)-3,4-dihydrocarbostyril and 6.0 g of morpholine were dispersed in 120 ml of dioxane and stirred at 60°-70° C. for 12 hours. The reaction mixture was concentrated under a reduced pressure. The residue thus obtained was stirred with ether and the insoluble matter was collected by filtration and washed with water. Then the insoluble matter was dissolved in 80 ml of methanol and 10 ml of concentrated hydrochloric acid by heating and the solution was concentrated under a reduced pressure to dryness. The residue thus obtained was recrystallized from methanol-ether twice and obtained 5.9 g of 6-(1-oxo-2-morpholinoethyl)-3,4-dihydrocarbostyril monohydrochloride in colorless powdery product.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under a reduced pressure
- customThe residue thus obtained
- filtrationthe insoluble matter was collected by filtration
- washwashed with water
- dissolutionThen the insoluble matter was dissolved in 80 ml of methanol
- temperature10 ml of concentrated hydrochloric acid by heating
- concentrationthe solution was concentrated under a reduced pressure to dryness
- customThe residue thus obtained
- customwas recrystallized from methanol-ether twice