Diethyl Ether → HCID 12833213, compound

Participants

Reaction Conditions

Reaction Steps

84 g (1.5 mols) of isobutylene and 10.0 g (0.099 mol) of triethylamine are heated in an autoclave to 120° C. A solution of 17.35 g (0.1 mol) of 4,4-dichlorobut-3-enecarboxylic acid chloride in 35 ml of diethyl ether is then injected in the course of 30 minutes, and the reaction mixture is stirred at 120° C. for 2 hours. After cooling, the reaction mixture is triturated with diethyl ether. Solid constituents are filtered off, and the filtrate is subsequently washed with 1 N sulphuric acid (2×30 ml) as well as with 1% sodium bicarbonate solution (3×50 ml). After drying over sodium sulphate, concentration by evaporation is performed, and the residue is distilled in a bulb tube to yield 2-(2',2'-dichlorovinyl)-3,3-dimethylcyclobutanone as colourless oil; b.p. 100°-110° C./0.5 Torr.

Provenance & Evidence