Hydrogen Peroxide → HCID 85565303, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 16.32 mL of 90% aqueous hydrogen peroxide (0.6 mole), 2.3 mL of deionized water and 18.17 mL of 95.5% sulfuric acid was formed in a 150 mL beaker equipped with an ice bath, alcohol thermometer and mechanical stirrer. The water and sulfuric acid were added sequentially to the H2O2 with cooling and stirring to hold the temperature of the mixture to about 25° C. This mixture was added to 18.215 g (0.1 mole) of sulfonyldiacetic acid in admixture with 100 mL of methylene chloride without cooling over a period of about 8 minutes with agitation. The resulting combination formed two liquid phases and one solid phase. Agitation of this mixture was continued for three hours with the temperature in the range of 20°-22° C. under cover to reduce loss of methylene chloride. The mixture was then cooled to about 5° C. and diluted with 18 mL of deionized water added gradually with stirring and cooling. The solids were collected, reslurried with methylene chloride and treated with 80 mL of 6% aqueous sodium bicarbonate. The solids were collected and similarly treated with another 40 mL of 6% NaHCOs resulting in a final pH of about 4. The recovered solids appeared reduced by the reslurry operations and were combined with 2.91 g of dry powdered boric acid. The mixed solids were dried to constant weight (5.24 g) and found to have an active oxygen content of 5.03%.

Provenance & Evidence