Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Trichloroacetyl chloride | HCID 6420 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2629-78-9 | HCID 10958312 | 64% |
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05831131 |
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| Source dataset | uspto-grants-1998_11 |
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| ORD ID | ord-fd4ee116584c4e34aafff3900352f90c |
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| Source note | uspto-grants-1998_11 |
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