HRID1590783
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 0.997 g (2.55 mmol) of the phthalimide prepared above, 124 microliters (2.55 mmol) of 98% hydrazine monohydrate, and 25 ml of ethanol is heated at reflux under N2 overnight. TLC (90:10 CHCl3 :CH3OH) of the reaction mixture showed some phthalimide still present. An additional 25 ml of hydrazine was added, and the mixture heated at reflux for 3 hrs. The solvent is removed under vacuum, the residue taken up in about 10 ml of CH3OH and flash chromatographed on silica gel (90:10:2 CHCl3 :CH3OH:NH4OH) to give 531 mg of 6-[4-(3-aminopropyloxy)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone as a white solid. Yield 80%.
WORKUP
后处理
- temperatureis heated
- temperatureat reflux under N2 overnight
- temperaturethe mixture heated
- temperatureat reflux for 3 hrs
- customThe solvent is removed under vacuum
- customflash chromatographed on silica gel (90:10:2 CHCl3 :CH3OH:NH4OH)