Hydrogen Peroxide → (2,2-dichloroacetyl) 2,2-dichloroethaneperoxoate

A beaker was loaded with 1.25 g of lithium hydroxide monohydrate (30 mmoles), 28 mL of water, 90 mL of Freon® 113, 3.07 mL of 30% aqueous hydrogen peroxide (30 mmoles), and finally 1.64 mL of dichloroacetyl chloride (17 mmoles) with ice bath cooling. An ultrasonic horn connected to a 40 Khz, 150 watt Dukane power source was immediately started up at 75% maximum power and lowered into the reaction mixture. After 15 seconds, the ultrasonic horn was turned off and the reaction mixture poured into a prechilled 250 mL Erlenmeyer flask sitting on dry ice. The reaction mixture was first allowed to freeze solid and then warmed with swirling. As soon as the Freon® 113 phase has thawed entirely to 90 mL of fluid, a 5.0 mL sample was drawn and found to take 4.5 mL of 0.1N sodium thiosulfate in iodometric titration (yield 48% based on starting dichloroacetyl chloride).

1. temperaturecooling
2. additionthe reaction mixture poured into a prechilled 250 mL Erlenmeyer flask
3. temperaturewarmed

ORD record

ord-c8f2fb1a326745b488c12afb77894fdd

Source dataset

uspto-grants-1998_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05831131