HRID1870742

反应详情

EQUATION

反应方程式

HRID 1870742 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-[N-(5-Bromo-2-(2-methylprop-2-en-1-yloxy)benzyl)-N-ethylamino]pyridazine-3-carboxamide (430 mg, 1.09 mmol) was dissolved in THF/methanol (30 ml, 1:1) and sodium hydroxide solution added (2.9 ml, 2M, 5.8 mmol). The mixture was heated at reflux for 72 hours, allowed to cool and evaporated. The residue was dissolved in water (25 ml) and acetic acid added to pH-4. The solution was stirred for 16 hours and then the resulting colourless precipitate collected by filtration, washed with water and dried under vacuum to give the title compound as a colourless powder (387 mg, 87%).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 72 hours
  3. temperatureto cool
  4. customevaporated
  5. dissolutionThe residue was dissolved in water (25 ml)
  6. additionacetic acid added to pH-4
  7. filtrationthe resulting colourless precipitate collected by filtration
  8. washwashed with water
  9. customdried under vacuum