Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Pinacolone | HCID 6416 | — |
| Reactant | Methanesulfenyl chloride, trifluoro- | HCID 67900 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 14144952 | HCID 14144952 | — |
Reaction Steps
A mixture of 3,3-dimethyl-2-butanone (1.13 mole), ethanol (1.5 g.) and dichloromethane (300 ml) was introduced into a sealed and pressure tested 2-liter vessel under reduced pressure. Trifluoromethanesulfenyl chloride (1.05 mole) was then added to the cooled, evacuated vessel. (Caution: It should be noted that trifluoromethanesulfenyl chloride is a highly hazardous material which must be handled with care to avoid inhalation and contact with the skin.) The vessel was warmed to about 25°C. and then rocked for 21/2 to 3 days. The vessel was vented through a cold gas trap (-78°C.) to trap any unreacted trifluoromethane sulfenyl chloride, and then through a scrubbing system to remove the vented hydrogen chloride gas. Residual liquid was transferred to a flask and distilled to give 1-trifluoromethylthio-3,3-dimethyl-2-butanone, b.p. 65°C./10mmHg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US03932508 |
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| Source dataset | uspto-grants-1976_01 |
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| ORD ID | ord-22fbee51cc4f4473b161471452c78734 |
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| Source note | uspto-grants-1976_01 |
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