HRID2371926
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 5.4 g (13.1 mmol) of the phthalimide prepared above and 700 microliters (14.4 mmol) of hydrazine monohydrate in 150 ml of isopropanol is heated at reflux overnight. The solvent is removed under vacuum, the residue is taken up in 15 ml of 70:30 (CH3OH:NH4OH) and flash chromatographed on silica gel (90:10:2 CHCl3 :CH3OH:NH4OH) to give 2.13 g of 6-[4-(3-aminopropyl)-3-chlorophenyl]-4,5-dihydro-3(2H)-pyridazinone as a pale yellow solid. Yield, 58%.
WORKUP
后处理
- temperatureis heated
- temperatureat reflux overnight
- customThe solvent is removed under vacuum
- customchromatographed on silica gel (90:10:2 CHCl3 :CH3OH:NH4OH)