Phosphorus oxychloride → HCID 86619138, compound

Participants

Reaction Conditions

Reaction Steps

1.69 g of the 6-oxo-2-{[(1S)-1-phenylethyl]amino}-1,6-dihydro-5-pyrimidinecarbonitrile [54-1] was dissolved in 100 mL of acetonitrile, then 5 mL of phosphorus oxychloride was added, and stirred at 85° C. for 2 hours. After concentrating the reaction mixture under reduced pressure, the obtained residue was placed in an ice bath, extracted with ethyl acetate, and the organic layer was washed with water and saturated brine in the subsequent order. After drying over anhydrous magnesium sulfate, the insolubles were filtered, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography, and 1.54 g of 4-chloro-2-{[(1S)-1-phenylethyl]amino}-5-pyrimidinecarbonitrile [54-2] was obtained as an oily product.

Provenance & Evidence