Acetone → HCID 178476249, compound

Participants

Reaction Steps

100 ml of methanol, 80 ml of acetone and 0.7 ml of concentrated hydrochloric acid were added to 10.0 g (28.1 mmol) of N1-hexyl-N5-heptyl-biguanide dihydrochloride. The mixture was refluxed for 23 hours, and the solvent was distilled off under reduced pressure. To the residue were added 100 ml of ethanol, 60 ml of water and 11.3 ml of 5N sodium hydroxide, and the mixture was refluxed for 1 hour, concentrated under reduced pressure, and extracted with ethyl acetate. The extract was washed successively with 10% aqueous sodium acetate and water, and the solvent was distilled off under reduced pressure. The residue was recrystallized from methyl ethyl ketone to obtain 8.4 g of colorless crystals having a melting point of 70 to 75° C.

Provenance & Evidence