Phosphorus oxychloride → HCID 86721466, compound

Participants

Reaction Conditions

Reaction Steps

[step 5] To (E)-2-{8-[(2-cyclopropyl-8-hydroxyimidazo[1,2-a]pyrazin-3-yl)methyl]-3-fluorodibenzo[b,e]oxepin-11(6H)-ylidene}propanenitrile (3.8 g, 8.3 mmol) obtained in step 4 was added phosphorus oxychloride (19 mL, 207 mmol), and the mixture was stirred with heating at 110° C. for 4 hr. The mixture was concentrated under reduced pressure, saturated aqueous sodium hydrogen carbonate solution was added to the residue, and the mixture was extracted 3 times with ethyl acetate. The combined organic layers were dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give (E)-2-{8-[(8-chloro-2-cyclopropylimidazo[1,2-a]pyrazin-3-yl)methyl]-3-fluorodibenzo[b,e]oxepin-11(6H)-ylidene}propanenitrile (3.7 g, 96%).

Provenance & Evidence