HRID1161531
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
CONDITIONS
反应条件
- 温度
- 62.5 °C
PROCEDURE
实验过程
To a solution of 68 mg of 5-(3-{(5-fluoro-8-methoxy-2,3-dihydrobenzo[1,4]dioxin-6-yl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]methyl}-5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl)-1H-pyrazole-4-carboxylic acid ethyl ester in 6 ml of a methanol:water:acetic acid=1:1:1 mixed solvent there was added 68 mg of iron powder, and the mixture was stirred at 62.5° C. for 40 hours under a nitrogen atmosphere. After cooling, the reaction mixture was filtered through celite and purified by reverse-phase high performance liquid chromatography (acetonitrile-water, 0.1% acetic acid). The title compound (16.0 mg) was obtained as a white solid.
WORKUP
后处理
- temperatureAfter cooling
- filtrationthe reaction mixture was filtered through celite
- custompurified by reverse-phase high performance liquid chromatography (acetonitrile-water, 0.1% acetic acid)