HRID1867781

反应详情

EQUATION

反应方程式

HRID 1867781 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,5-Dinitro-benzoic acid 2-(2-bromo-2-methyl-propionyloxy)-ethyl ester (9 g, 0.022 mol) was dissolved in 100 ml ethanol/tetrahydrofuran (1:1). In succession, 10N HCl (27 ml, 0.27 mol) and tin(II)chloride (50.1 g, 0.22 mol) were added. The solution was stirred at room temperature 18 h. The reaction mixture was poured into a separatory funnel containing 100 ml ice-cold water followed by the addition of 20% KOH (ice-cold, 444 g). The mixture was extracted with ether (3×100 ml). The combined organic phases were washed with water (3×100 ml) and brine, dried with solid MgSO4 and concentrated to 5.6 g.

WORKUP

后处理

  1. additionThe reaction mixture was poured into a separatory funnel
  2. extractionThe mixture was extracted with ether (3×100 ml)
  3. washThe combined organic phases were washed with water (3×100 ml) and brine
  4. dry with materialdried with solid MgSO4
  5. concentrationconcentrated to 5.6 g