Ethanol → HCID 14144952, compound

Temperature

25 °C

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.

1. additionwas introduced into
2. customa sealed
3. customevacuated vessel
4. custom2 to 3 days
5. customThe vessel was vented through a cold gas trap
6. custom(-78°C.) to trap any unreacted trifluoromethane sulfenyl chloride, and then through a scrubbing system to remove the vented hydrogen chloride gas
7. customResidual liquid was transferred to a flask
8. distillationdistilled

ORD record

ord-22fbee51cc4f4473b161471452c78734

Source dataset

uspto-grants-1976_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03932508