Hydrochloric Acid → HCID 22557326, compound

Participants

Reaction Steps

A solution of compound (36) (0.00425 mol) in THF (20 ml) was added dropwise at 5° C. to NH4OH (20 ml) and the mixture was stirred at RT for 2 hours, then poured out on ice, neutralized with HCl 6N and extracted with EtOAc. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 97/3). The pure fractions were collected and the solvent was evaporated. The residue was repurified by column chromatography over Kromasil C18 (eluent: CH3OH/H2O/HOAc 70/30/1). The pure fractions were collected and the solvent was evaporated. The residue was taken up in H2O and NH4OH (pH=8) was added. The precipitate was filtered off, washed with H2O and diethyl ether, and dried, yielding 0.3 g (±)-2-[3-chloro-4-[amino-(4-chlorophenyl)-2-thiazolylmethyl]phenyl]-1,2,4-triazine-3,5(2H,4H)-dione (compound 35).

Provenance & Evidence