Phosphorus oxychloride → HCID 86626009, compound

Participants

Reaction Conditions

Reaction Steps

Phosphorus oxychloride (15 mL) was added to 5-(5-cyclopropyl[1,3,4]oxadiazol-2-yl)-4-hydroxy-2-methylthiopyrimidine (6.26 g) obtained in Step 6, and the mixture was stirred at 60° C. for 30 minutes. After completion of the reaction was confirmed by thin-layer chromatography, the reaction mixture was added to a saturated aqueous sodium hydrogencarbonate solution, and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure. Diethyl ether was added to the residue to precipitate crystals. The resulting crystals were collected by filtration and dried thoroughly under reduced pressure to give 4-chloro-5-(5-cyclopropyl[1,3,4]oxadiazol-2-yl)-2-methylthiopyrimidine (5.31 g, yield 79%).

Provenance & Evidence