Sodium Thiosulfate → HCID 86662317, compound

Participants

Reaction Steps

6-Chloro-4-(5-(1-hydroxy-2-methylpropan-2-yloxy)pyridine-2-ylamino)-2-methylpyridazin-3-(2H)-one (965 mg, 2.97 mmol) was taken up in a mixture of tetrahydrofuran (25 ml) and dichloromethane (15 ml). To the suspension was added Dess-Martin Periodinane (1.64 g, 3.86 mmol) and the flask was capped and stirred for 40 minutes. An aqueous saturated solution of sodium bicarbonate (50 ml) followed by the addition of an aqueous 10% solution of sodium thiosulfate (50 ml) and the material was stirred vigorously for 15 minutes. Ethyl acetate (50 ml) was added and the contents were shaken in a separatory funnel. The organic phase was collected and washed with brine solution (50 ml). The ethyl acetate phase was collected and the aqueous phases were back extracted with dichloromethane (2×40 ml). The combined organic phases were dried over magnesium sulfate, filtered and concentrated in vacuo. The product was purified via trituration from hot dichloromethane/hexanes to provide a brown solid (688 mg) (M+H)+=323 m/e.

Provenance & Evidence