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

Temperature

0 °C

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.

1. filtrationThe reaction mixture is filtered through a pad of Drierite® on glass wool
2. washwashing through with fresh CFC-113
3. washThe peroxide solution is washed three times with ˜60 ml of water
4. washThe water wash may
5. customhave removed residual inorganic peroxide
6. filtrationmissed by the Drierite® filtration
7. customwas destroyed by hydrolysis

ORD record

ord-93bc5912c8ce4d26ae8fa522767abb5a

Source dataset

uspto-grants-2006_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07112314B2