[OH2:1].[OH-:2].[Li+].OO.[Cl:6][CH:7]([Cl:11])[C:8](Cl)=[O:9].S([O-])([O-])(=O)=S.[Na+].[Na+]>O>[Cl:6][CH:7]([Cl:11])[C:8]([O:1][O:2][C:8](=[O:9])[CH:7]([Cl:11])[Cl:6])=[O:9]
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).
Wird geladen…
