1-Methylpiperazine → HCID 13298530, compound

Participants

Reaction Steps

A solution of 2-chloro-3-fluoropyridine (1.0 g, 8.5 mmol) and N-methyl piperazine (4.26 g, 42.5 mmol) in n-butanol, 50 ml, is stirred at reflux for 18 hours. After concentrating under reduced pressure at 50° C., the residue is partitioned between ethyl ether and 50% NaOH solution. The ethyl ether extract is washed with a saturated sodium chloride solution, dried over Na2SO4, filtered and concentrated under reduced pressure. The oily product is converted to the hydrogen fumarate salt, mp 148°-149° C., by treatment with fumaric acid in methanol and precipitation with ethyl ether.

Provenance & Evidence