HCID 76492969, compound → HCID 53673207, compound

Participants

Reaction Steps

A mixture of intermediate (3d) (0.0069 mol) in HCl conc. (50 ml) was stirred and refluxed for 48 hours. The solvent was evaporated and the residue was dissolved in H2O (50ml). The mixture was alkalized with NH4OH and extracted with CH2Cl2/CH3OH 80/20 (500 ml). The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was triturated in 2-propanol, filtered off and dried, yielding 2.6 g (92%) of [R(R*,S*)]-2-(2-amino-1-methylpropyl)-2,4-dihydro-4-[4-[4-(4-hydroxyphenyl)-1-piperazinyl]phenyl]-3H-1,2,4-triazol-3-one (interm. 4; mp. 237.2° C.; [α]20D=+1.010° @19.79 mg/2ml in DMF).

Provenance & Evidence