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 comprising 11.58 g of 3-[3-(4-formylpiperazin-1-yl)-propoxy]-4-methoxybenzylamine, 5.0 g of 4,5-dichloro-3(2H)-pyridazinone, 4.6 g of triethylamine, 50 ml of n-propanol and 50 ml of water, was refluxed under heating with stirring for 14 hours. The solvent was distilled off under reduced pressure, and an aqueous potassium carbonate solution was added to the obtained residue, and the mixture was extracted with chloroform. The organic layer was washed with water and a saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate. Then, the solvent was distilled off, and the residue was purified by silica gel column chromatography to obtain 6.21 g of the above-identified compound as slightly yellow white solid.
WORKUP
后处理
- temperaturewas refluxed
- temperatureunder heating
- distillationThe solvent was distilled off under reduced pressure
- additionan aqueous potassium carbonate solution was added to the obtained residue
- extractionthe mixture was extracted with chloroform
- washThe organic layer was washed with water
- dry with materiala saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate
- distillationThen, the solvent was distilled off
- customthe residue was purified by silica gel column chromatography