Trifluoroacetic acid → HCID 86721453, compound

Participants

Reaction Conditions

Reaction Steps

[step 4] (E)-2-{8-[(2-cyclopropyl-8-methylimidazo[1,2-a]pyrazin-3-yl)(hydroxy)methyl]-3-fluorodibenzo[b,e]oxepin-11(6H)-ylidene}propanenitrile (18 g, 39 mmol) obtained in step 3 was dissolved in trifluoroacetic acid (181 mL, 2.3 mol), triethylsilane (31 mL, 0.19 mol) was added, and the mixture was stirred with heating at 60° C. for 1 hr. The mixture was concentrated under reduced pressure, saturated aqueous sodium hydrogen carbonate solution (100 mL) was added to the obtained residue, and the mixture was extracted 3 times with a mixed solvent of chloroform-methanol. The combined organic layers were dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. To the obtained residue was added isopropylalcohol (133 mL), and the mixture was stirred at room temperature for 4 hr and further for 1 hr under ice-cooling. The precipitated crystals were collected by suction filtration to give the title compound (13g, 72%).

Provenance & Evidence