Potassium Carbonate → HCID 178504863, compound

Participants

Reaction Steps

The mixture of (2,3-dihydro-9-methylthiomethyl-1-benzoxepin-4-carbonyl)guanidine (0.4 g) and m-chloroperbenzoic acid (0.52 g) in chloroform (20 ml) and methanol (4 ml) was stirred at ambient temperature for 2 hours. The reaction mixture was added to 10% aqueous sodium thiosulfate, adjusted to pH 9 with 20% aqueous potassium carbonate and extracted with a mixture of ethyl acetate and tetrahydrofuran. The extract layer was washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue was dissolved in methanol (5 ml), and methanesulfonic acid (0.11 ml) was added with stirring. To the mixture was added diisopropyl ether (5 ml) and isolated crystalline was collected by filtration. The crystalline was recrystallized from a mixture of methanol and diisopropyl ether to give (2,3-dihydro-9-methanesulfonylmethyl-1-benzoxepin-4-carbonyl)guanidine methanesulfonate (0.16 g).

Provenance & Evidence