HRID1590791

反应详情

EQUATION

反应方程式

HRID 1590791 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureis heated
  2. temperatureat reflux overnight
  3. customThe solvent is removed under vacuum
  4. customchromatographed on silica gel (90:10:2 CHCl3 :CH3OH:NH4OH)