Ammonia → HCID 70357805, compound

Participants

Reaction Conditions

Reaction Steps

12.5 g of pyridine hydrochloride and 5.2 g (12 mMol) of the compound of example 3 are mixed at room temperature, and heated to 160° C. whilst stirring. After 1 hour, a further 12.5 g of pyridine hydrochloride are added, and heating continues for a further hour at 160° C. After cooling, the mixture is taken up in ice water, rendered basic with conc. ammonia and extracted three times with methylene chloride. The organic phases are dried over Na2SO4, concentrated by evaporation and flash-chromatographed over silica gel with ethyl acetate/hexane 1:3. The following are isolated: the title compound as a colorless oil and unreacted starting material. The title compound is converted into the hydrochloride with ether/ethanol/HCl: M.p.: 260° C.

Provenance & Evidence