HRID1389998

反应详情

EQUATION

反应方程式

HRID 1389998 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
67 °C

PROCEDURE

实验过程

To 1.95 g (10 m moles) of 3-hydrazino-6-morpholino-pyridazine dissolved in 12 ml of acetic acid, 1.71 g (12 m moles) of 3,6-octanedione dissolved in 4 ml of acetic acid are added at room temperature. The mixture is heated at 67° C. for 2 hours and then evaporated to dryness under vacuum. The oily residue is dissolved in toluene and the solution is evaporated to dryness. The residue is slurried with ice-water and neutralized with sodium bicarbonate to yield 2.58 g of a solid product. Said material, after crystallization from isopropanol gives 1.25 g (42%) of the title product, melting at 186°-9° C. Elemental analysis, I. R., N.M.R. and mass spectra are in agreement with the assigned structure.

WORKUP

后处理

  1. additionare added at room temperature
  2. customevaporated to dryness under vacuum
  3. dissolutionThe oily residue is dissolved in toluene
  4. customthe solution is evaporated to dryness