Hydrochloric Acid → HCID 66751231, compound

Participants

Reaction Steps

To a stirred solution of 5-[(3-[1,3]dioxolan-2-yl-2,4-difluoro-phenylamino)-methyl]-imidazole-1-sulfonic acid dimethylamide (0.53 g, 1.27 mmol) in tetrahydrofuran (10 ml) was added a 4 N solution of hydrogen chloride in dioxane (3.87 ml, 15.5 mmol) and the mixture was stirred at room temperature for 24 h. The mixture was then concentrated in vacuo and the residue taken up in dichloromethane/methanol (95:5) and washed with 1 N aq. sodium hydroxide solution. The layers were separated and the aqueous phase was back extracted twice with dichloromethane/methanol (95:5). The combined organic phases were washed with saturated brine, then dried over magensium sulfate and concentrated in vacuo. The residue was purified by flash chromatography (column: Isolute® Flash-NH2 (Separtis); eluent: methanol/dichloromethane gradient) to yield a colourless gum (225 mg, 57%); MS (ISP): 310.3 ((M+H)+.).

Provenance & Evidence