HRID588267

反应详情

EQUATION

反应方程式

HRID 588267 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customwas removed by filtration
  2. concentrationThe filtrate was concentrated
  3. additionH2O was added to the residue
  4. extractionextracted with CHCl3
  5. dry with materialThe organic layer was dried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. customPurification by column chromatography (CHCl3/MeOH)