Sulfuric Acid → HCID 78103722, compound

Participants

Reaction Conditions

Reaction Steps

To 780 mg (1.97 mmol) [(3-{[3-(1-benzofuran-2-yl)imidazo[1,2-b]pyridazin-6-yl]oxy}propyl)(methyl)oxido-lambda6-sulfanylidene]cyanamide were added 20 mL 50% aqueous sulfuric acid. It was stirred 2 hours at 140° C. bath temperature. The reaction was allowed to reach room temperature. The sulfuric acid was diluted with 20 mL water and the pH was adjusted to 12 with 50% aqueous sodium hydroxide on an ice bath. The aqueous phase was extracted with 30 mL dichloromethane. During the second extraction water had to be added to separate the layers. The first organic phase was combined with the reaction mixture and vigorously shaken. The layers were separated and the aqueous phase was extracted three times with dichloromethane. The combined organic layers were dried over sodium sulfate and concentrated yielding 530 mg (72%) of a yellow solid.

Provenance & Evidence