Methyl Bromide → HCID 69958772, compound

Participants

Reaction Steps

In 5 ml of chloroform were dissolved 0.34 g of 4-(1,2,3,4-tetrahydrobenzo[b]thieno[2,3-c]pyridine-3-carbonyl)morpholine hydrochloride, 0.31 ml of triethylamine, and 0.11 g of methyl bromide, and the solution was refluxed for 30 minutes. Chloroform was distilled off under reduced pressure, 20 ml of an aqueous 5% sodium hydrogencarbonate solution and 50 ml of ethyl acetate were added to the residue, and the ethyl acetate layer was washed with a saturated sodium chloride solution and dried by sodium sulfate. Then, ethyl acetate was distilled under reduced pressure and the residue was purified by silica gel thin layer chromatography. Then, 1 ml of a mixture of 1N hydrochloric acid in ethyl acetate was added to the residue and crystals deposited were collected by filtration to provide 0.29 g (yield of 82%) of 4-(2 -methyl-1,2,3,4-tetrahydrobenzo[b]thieno[2,3-c]pyridine-3-carbonyl)morpholine.hydrochloride.

Provenance & Evidence