Cfc 113 → Peroxide, bis(2-methyl-1-oxopropyl)
反応式
[C:1]([O-:4])([O-])=O.[C:5]([O-])([O-])=O.[OH:9][OH:10].OO.OO.[Na+].[Na+].[Na+].[Na+].[C:19](Cl)(=[O:23])[CH:20]([CH3:22])[CH3:21].[C:25](Cl)(F)(F)[C:26](Cl)(Cl)F>>[C:19]([O:9][O:10][C:1](=[O:4])[CH:25]([CH3:26])[CH3:5])(=[O:23])[CH:20]([CH3:22])[CH3:21]参加物
4
反応条件
- 温度
- 0 °C
実験手順
A round-bottom flask is charged with 50 ml of CFC-113 and 2.0 g of sodium percarbonate (13 mmoles or 19 mmoles of H2O2 equivalent). After chilling the contents of the flask to 0° C., 2.60 ml of isobutyryl chloride (25 mmoles) is added and the resulting slurry is stirred magnetically for 223 minutes. The reaction mixture is filtered through a pad of Drierite® on glass wool, washing through with fresh CFC-113. The filtrate, now measuring 59 ml in volume, is found to be 0.083 M in peroxide, which is a 39% yield based on starting isobutyryl chloride. The peroxide solution is washed three times with ˜60 ml of water. The washed solution is retitrated and found to be 0.050 M in peroxide. The water wash may have removed residual inorganic peroxide missed by the Drierite® filtration, but is more likely that some of the isobutyryl peroxide was destroyed by hydrolysis.