HRID1603625

反应详情

EQUATION

反应方程式

HRID 1603625 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.79 g (0.002 mol) of N-[3-bromo-5-(4-nitrophenylsulphanyl) -phenyl]-N-methylacetamide was dissolved in a mixture of 10 ml of dioxane and 10 ml of 1N NaOH and heated at reflux for 2 hrs. Subsequently, the organic solvent was distilled off and the residue was made neutral with 1N HCl and extracted with ethyl acetate. The organic phase was washed with water and sat. sodium chloride solution, dried over MgSO4, filtered, concentrated and dried. There was obtained 0.723 g (100%) of [3-bromo-5-(4-nitrophenylsulphanyl)-phenyl]-methylamine as red crystals; m.p.: 96-98° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 2 hrs
  3. distillationSubsequently, the organic solvent was distilled off
  4. extractionextracted with ethyl acetate
  5. washThe organic phase was washed with water and sat. sodium chloride solution
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customdried