Methanesulfonic Acid → HCID 54492772, compound

Participants

Reaction Steps

To a solution of 6.2 g of 4-amidino-2-methoxyphenol methanesulfonate in 30 ml of dried pyridine, while being cooled in ice and stirred, was added 3.9 g of cinnamoyl chloride. Immediately after the addition a colorless solid substance precipitated from the reaction mixture. After 3 hours of stirring at room temperature, ethyl ether was added to the mixture and the precipitate was collected by filtration. The precipitate was dissolved in methanol and mixed with a saturated aqueous sodium bicarbonate solution to precipitate a white gelatinous substance. The gelatinous substance was collected by filtration, washed with water, then with acetone and dried to obtain 6.3 g of the carbonate of the captioned compound. Upon addition of 2.3 g of methanesulfonic acid to the carbonate suspended in 60 ml of methanol, a change in crystal form of the carbonate took place accompanied by effervescence. The suspension was heated to dissolve the crystals and then cooled to obtain 6.3 g of colorless needle crystals of 4-amidino-2-methoxyphenyl cinnamate methanesulfonate.

Provenance & Evidence