HRID442741

反应详情

EQUATION

反应方程式

HRID 442741 的结构方程式

PROCEDURE

实验过程

Under an inert atmosphere, 1.9 g of the previous compound are dissolved in 20 ml of anhydrous ethyl acetate and 5 ml of anisole and 20 ml of a 5N solution of HCl in ethyl acetate are added slowly at 5° C. The mixture is allowed to attain room temperature and after being stirred for 2 hours is cooled to about 5° C. before a 5N aqueous solution of NaOH is added to give a basic pH. The organic phase is then separated, dried and concentrated at about 70° C. under reduced pressure. The residual oil is dissolved in 60 ml of isopropanol and decolorized by means of 50 mg of active charcoal and 50 ml of a 0.5M solution of oxalic acid dihydrate in isopropanol are added; the precipitated salt is isolated by filtration. 1.5 g of oxalate hemihydrate are thus obtained (containing two molecules of oxalic acid), M.p.=130° C.

WORKUP

后处理

  1. customto attain room temperature
  2. additionis added
  3. customto give a basic pH
  4. customThe organic phase is then separated
  5. customdried
  6. concentrationconcentrated at about 70° C. under reduced pressure
  7. dissolutionThe residual oil is dissolved in 60 ml of isopropanol
  8. additionare added
  9. customthe precipitated salt is isolated by filtration