Hydrogen Peroxide → 2629-78-9

Lithium Hydroxide as Base. 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, and finally 1.9 ml of trichloroacetyl 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 had thawed entirely to 88 ml of fluid, a 5.0 ml sample was drawn and found to take 6.2 ml of 0.1N sodium thiosulfate in iodometric titration (yield 64% based on starting trichloroacetyl chloride).

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

ORD record

ord-fd4ee116584c4e34aafff3900352f90c

Source dataset

uspto-grants-1998_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05831131