HRID1870742
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
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
- temperatureThe mixture was heated
- temperatureat reflux for 72 hours
- temperatureto cool
- customevaporated
- dissolutionThe residue was dissolved in water (25 ml)
- additionacetic acid added to pH-4
- filtrationthe resulting colourless precipitate collected by filtration
- washwashed with water
- customdried under vacuum