Potassium Carbonate → HCID 71535015, compound

Participants

Reaction Steps

25 mL methanol were added to 1 g (2.64 mmol) [(3-{[3-(1-benzofuran-2-yl)imidazo[1,2-b]pyridazin-6-yl]oxy}propyl)(methyl)-lambda4-sulfanylidene]-cyanamide in 20 mL dichloromethane. To the clear solution 25 mL ethanol were added. 6.614 g (5.27 mmol) potassium peroxymonosulfate were dissolved in 24 mL water. 2.186 g (15.82 mmol) potassium carbonate were dissolved in 16 mL water and transferred to the potassium peroxymonosulfate solution. This solution was added in 40 min under vigorous stirring. After 19 h 200 mL dichloromethane and 50 mL of a saturated sodium thiosulfate solution was added and stirred for a few minutes. The layers were separated and the aqueous phase was extracted three times with 50 mL dichloromethane. The combined organic layers were dried over sodium sulfate, and concentrated. This residue was dissolved in 20 mL dichloromethane and 25 mL methanol. To the clear solution 25 mL ethanol were added. 6.61 g (5.27 mmol) potassium peroxymonosulfate were dissolved in 24 mL water. 2.19 g (15.85 mmol) potassium carbonate were dissolved in 16 mL water and transferred to the potassium peroxymonosulfate solution. This solution was added in 15 minutes under vigorous stirring. After 4 hours 200 mL dichloromethane and 30 mL of a saturated sodium thiosulfate solution was added and stirred for a few minutes. The layers were separated and the aqueous phase was extracted once with 50 mL dichloromethane. The combined organic layers were dried over sodium sulfate, and concentrated to yield 0.98 g (94%) of a yellow solid.

Provenance & Evidence