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 solution of 1-(3-chloropropyl)-5,6-dihydro-(1H,4H)-1,2,5-thiadiazolo[4,3,2-ij]quinoline 2,2-dioxide (4 g), 4-(4-hydroxyphenyl)piperazine (4.75 g) and triethylamine (5.88 cc) in dry N,N-dimethylformamide (50 cc) is heated to reflux for 90 minutes and is then cooled and poured into a mixture of water (300 cc) and ethyl acetate (300 cc). The organic phase is washed with water (3×200 cc), is dried over magnesium sulphate and is concentrated to dryness under reduced pressure (2.7 kPa). The solid is recrystallized from ethyl acetate (300 cc) and dried. 1-[3-(4-(4-Hydroxyphenyl)-1-piperazinyl)propyl]-5,6-dihydro(1H,4H)-1,2,5-thiadiazolo[4,3,2-ij]quinoline 2,2-dioxide (2.8 g) is obtained, melting at 182° C.
WORKUP
后处理
- temperatureto reflux for 90 minutes
- temperatureis then cooled
- washThe organic phase is washed with water (3×200 cc)
- dry with materialis dried over magnesium sulphate
- concentrationis concentrated to dryness under reduced pressure (2.7 kPa)
- customThe solid is recrystallized from ethyl acetate (300 cc)
- customdried