3-Chloro-2-butanone → HCID 12959396, compound

Participants

Reaction Steps

5.0 gm (0.015 mol) of 2-(2,6-dibromo-4-methyl-phenylimino)-imidazolidine were refluxed for about 30 hours with 1.8 gm (110%) of 96% 3-chloro-2-butanone in 25 ml of glycol monomethyl ether. The reaction mixture was then evaporated to dryness in vacuo, and the oily residue was dissolved in 1 N hydrochloric acid. The hydrochloric acid solution was adjusted to a pH value of 7 with dilute NaOH and, starting from the pH value, was fractionally extracted with ether at increasing pH values (NaOH). The ether extracts which were uniform according to thin-layer chromatography were combined, dried over magnesium sulfate, and the ether was eliminated in vacuo. The residual oil crystallized out after a short time. Yield: 0.4 gm of the compound of the formula ##STR10## corresponding to 7% of theory. Melting point: 154°-156° C.

Provenance & Evidence