Cfc 113 → Peroxide, bis(2-methyl-1-oxopropyl)

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

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.

Herkunft & Nachweise