HRID1106870

反应详情

EQUATION

反应方程式

HRID 1106870 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 11 g (0.040 mol) of the 1-(2-chloro-4-nitrophenoxy)-2-bromoethane produced in Example 5-(1), ethanol (170 ml) was added and dissolved therein; to the resulting solution, Na2S2O4 (27.6 g, 0.158 mol) as dissolved in water (50 ml) was added dropwise, followed by stirring at room temperature for 20 min. The solvent was evaporated and the residue was diluted with an aqueous solution of sodium bicarbonate and two extractions were conducted with ethyl acetate. The organic extracts were dried with sodium sulfate and the solvent was evaporated, with the residue being purified by being subjected to column chromatography on silica gel using, as an eluent, n-hexane containing ethyl acetate (25%) to yield the end compound 1-(4-amino-2-chlorophenoxy)-2-bromoethane (2.35 g) as a pale yellow solid mass.

WORKUP

后处理

  1. dissolutiondissolved
  2. additionwas added dropwise
  3. customThe solvent was evaporated
  4. additionthe residue was diluted with an aqueous solution of sodium bicarbonate and two extractions
  5. dry with materialThe organic extracts were dried with sodium sulfate
  6. customthe solvent was evaporated, with the residue
  7. custombeing purified
  8. additionn-hexane containing ethyl acetate (25%)