Sulfate Ion → HCID 86759321, compound

Participants

Reaction Conditions

Reaction Steps

4.5 kg (32.6 mol) of potassium carbonate were suspended in 3.2 1 of methyl tert-butyl ether and one liter of DMF in a 20 l vessel. The mixture was cooled to 0 to −10° C. with stirring. A solution of 4128 g (32 mol) of pentane-2,3,4-trione 3-oxime, 2 l of DMF and 4032 g (32 mol) of diemethyl [sic] sulfate was then metered in over the course of 2 hours at an internal temperature of <25° C. The mixture was then stirred at room temperature for 3.5 hours. 20 l of water was subsequently metered in, the upper organic phase was separated off, the aqueous phase was washed with 2 l of methyl tert-butyl ether, the combined organic phase were washed with 1 l of 5% strength hydrochloric acid, and the solvent was distilled off. 4214 g of the title compound were obtained in a purity of 96.6% (GC percent area) which corresponds to a yield of 89%.

Provenance & Evidence