Ethylene Glycol → HCID 21313213, compound

Participants

Reaction Steps

57 Parts of 1-(5-chloro-2-thienyl)-1-ethanone are dissolved in 220 parts of 1,2-ethanediol at 50° C. While stirring, there are added dropwise, during a 1 hour-period, 64 parts of bromine without external heating. After stirring for 1 hour at room temperature, 4 parts of 4-methylbenzenesulfonic acid and 360 parts of benzene are added. The whole is stirred and refluxed overnight with water-separator. The reaction mixture is evaporated and the residue is taken up in 2,2'-oxybispropane. The resulting solution is washed successively once with a diluted sodium hydroxide solution and three times with water, dired, filtered and evaporated. The residue is distilled, yielding 73.3 parts (64.5%) of 2-(bromomethyl)-2-(5-chloro-2-thienyl)-1,3-dioxolane; bp. 125°-127° C. at 0.1 mm. pressure.

Provenance & Evidence