HCID 70593817, compound → HCID 70598459, compound

Participants

Reaction Steps

5 gm (0.02 mol) of 7-(2-chloro-6-methyl-phenyl)-5-hydroxy-2,3,5,6-tetrahydro-imidazo[1,2-α]-imidazole were slowly heated to 180° C. on an oil bath, while stirring, and allowed to remain at that temperature for about 5 minutes. The molten mass was allowed to cool, was then dissolved in dilute hydrochloric acid, and the solution was extracted once with ether. The ethereal extract solution was discarded. The acidic aqueous phase was made alkaline with 2 N sodium hydroxide and was then extracted several times with ether while salting out (common salt). The combined ethereal extracts were dried over anhydrous calcium sulfate and evaporated in vacuo, leaving 2.9 gm (63% of theory) of slightly impure reaction product, as determined by thin-layer chromatography. For further purification the product was twice stirred with ether and suction-filtered off, yielding 1.1 gm (23.9% of theory) of 7-(2-chloro-6-methyl-phenyl)-2,3-dihydro-imidazo[1,2-α]-imidazole, m.p. 105°-107° C.

Provenance & Evidence