Sodium Chloride → Cyclopropanecarboxylic acid, 3-(2,2-dichloroethenyl)-2,2-dimethyl-, ethyl ester

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Reaction Steps

30 g (0.1 mol) of 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropane-1,1-dicarboxylic acid diethyl ester, 50 ml of 1-oxo-1-methyl-phospholine, 6 g of sodium chloride and 4 ml of water were heated to 175° C. for 9 hours. The mixture was then cooled, poured into 150 ml of water and extracted with petroleum ether. After drying with MgSO4, the mixture was fractionally distilled. 21.3 g (=90% of theory) of 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropane-1-carboxylic acid ethyl ester of boiling point 65°-75° C./0.1 mm Hg were obtained. 49.7 g of 1-oxo-1-methyl-phospholine of boiling point 75°-77° C./0.15 mm Hg were recovered by fractional distillation of the aqueous phase.

Provenance & Evidence