Water → HCID 15952855, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 1-{[6-chloro-2-(trifluoromethyl)imidazo[1,2-b]pyridazin-3-yl]methyl}-4-propylpyrrolidin-2-one 30 (400 mg, 1.11 mmol) and sodium methanethiolate (155 mg, 2.22 mmol, 2.2 eq) in THF is heated in a microwave apparatus (300 W, Tmax 150° C.) during 15 minutes. After cooling to room temperature, hydrolysis (15 ml of water), extraction (ethyl acetate, 3×15 ml), the cumulated organic layers are dried over MgSO4, filtered and condensed under reduce pressure to afford an oil which is purified under preparative chromatography over silicagel (Gradient: CH2Cl2 to CH2Cl2/MeOH/NH4OH 99/1/0.1 (v/v/v)). Recrystallization in diisopropyl ether affords 1-{[6-(methylthio)-2-(trifluoromethyl)imidazo[1,2-b]pyridazin-3-yl]methyl}-4-propylpyrrolidin-2-one 46.

Provenance & Evidence