HCID 12659681, compound → HCID 23330247, compound

Participants

Reaction Conditions

Reaction Steps

18 g of 1-chloro-1-(2',2',2'-trichloroethyl)spiro(3.3)-heptan-2-one is placed into 200 ml of formic acid, and 8.5 g of zinc dust is added portionwise in such a way that the temperature does not exceed 30° C. The reaction mixture is afterwards stirred for two hours at 30° C. and then filtered. The filtrate is concentrated by evaporation; water is added and the mixture is extracted with diethyl ether. The ethereal phase is washed with water, with aqueous sodium carbonate solution and again with water; it is dried over sodium sulphate and concentrated by evaporation. The residue is distilled at 75°-80° C./0.03-0.05 Torr to yield 1-(2',2',2'-trichloroethyl)spiro(3.3)heptan-2-one of the formula ##STR12## as a clear liquid.

Provenance & Evidence