HRID2371096

反应详情

EQUATION

反应方程式

HRID 2371096 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of the compound 1,2,3-benzotriazin-4(3H)-one (500 mg) (commercially available) in dimethylformamide (13 ml) was added anhydrous potassium carbonate (2.8 g) and stirred for 20 minutes. To it was added dibromoethane (2 g) and stirred the reaction mixture first at room temperature for few minutes and then at 60° C. for 2 hours. The solid thus obtained was filtered and the filterate was concentrated under reduced pressure. The residue thus obtained was diluted with water and extracted with ethylacetate. The organic layer was separated, washed with water and brine and dried over anhydrous sodium sulphate. The solvent was evaporated under reduced pressure and the residue thus obtained was purified by column chromatography using 20% ethyl acetate in hexane as eluant to furnish the title compound (590 mg).

WORKUP

后处理

  1. stirringstirred the reaction mixture first at room temperature for few minutes
  2. waitat 60° C. for 2 hours
  3. customThe solid thus obtained
  4. filtrationwas filtered
  5. concentrationthe filterate was concentrated under reduced pressure
  6. customThe residue thus obtained
  7. extractionextracted with ethylacetate
  8. customThe organic layer was separated
  9. washwashed with water and brine
  10. dry with materialdried over anhydrous sodium sulphate
  11. customThe solvent was evaporated under reduced pressure
  12. customthe residue thus obtained
  13. customwas purified by column chromatography