HRID1005623

反应详情

EQUATION

反应方程式

HRID 1005623 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

64.0 g of 35% sodium octyl sulfate (Aldrich, Milwaukee, Mich.) in water was slowly added in 31.0 g of 2-methoxy-4-(phenylamino)-benzenediazonium bisulfate (Diverstec, Fort Collins, Colo.) in 500 ml of water while stirring. The mixture was stored in dark at 0-5° C. for 5 hours. After decanting water, the resulting oil material was dissolved in 200 ml ethyl acetate. The solution was washed with 50 ml of 5% NaHCO3 and then with 50 ml of water. The organic layer was dried over anhydrous MgSO4 for 6 hours, and the solvent was removed by vacuum. 35.1 g of oil material was obtained.

WORKUP

后处理

  1. customdark at 0-5° C.
  2. customfor 5 hours
  3. customAfter decanting water
  4. dissolutionthe resulting oil material was dissolved in 200 ml ethyl acetate
  5. washThe solution was washed with 50 ml of 5% NaHCO3
  6. dry with materialThe organic layer was dried over anhydrous MgSO4 for 6 hours
  7. customthe solvent was removed by vacuum