HRID588267
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
- 150 °C
PROCEDURE
实验过程
To a solution of 2-oxoindoline-5-carbohydrazide (200 mg, 1.05 mmol) in n-BuOH/DMF (6 ml/2 ml) was added benzonitrile (324 mg, 3.14 mmol) and potassium carbonate (29 mg, 0.21 mmol). The mixture was heated at 150° C. for 3 hours under microwave irradiation. CHCl3/MeOH (20 ml/1 ml) was added to the mixture and insoluble solid was removed by filtration. The filtrate was concentrated. H2O was added to the residue and extracted with CHCl3. The organic layer was dried over Na2SO4 and concentrated in vacuo. Purification by column chromatography (CHCl3/MeOH) gave 5-(3-phenyl-1H-1,2,4-triazol-5-yl)indolin-2-one (15 mg).
WORKUP
后处理
- customwas removed by filtration
- concentrationThe filtrate was concentrated
- additionH2O was added to the residue
- extractionextracted with CHCl3
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated in vacuo
- customPurification by column chromatography (CHCl3/MeOH)