Hydrochloric Acid → HCID 70156360, compound

Participants

Reaction Steps

1-(4-Chlorophenylsulphonyl)-4-[1-(2,6-dimethylpyrimidin-4-yl)-4-piperidylcarbonyl]piperazine (603 mg, 0.96 mol) was refluxed in THF (5 ml), borane-dimethyl sulphide complex was added continuously and reflux continued for 4 hours. Reaction was stirred over a weekend to a residue. THF (5 ml) was added followed by 0.2 μL 6M HCl and stirred for 6 hours. Reaction basified by addition of dilute NaOH and partitioned between DCM and H2O. Organic layer was sepearted and dried in vacuo affording a white solid. Further purification by filtration column chromatography (silica) DCM to 10% MeOH/DCM and concentration of relevant fractions afforded 1-(4-chlorophenylsulphonyl)-4-[1-(2,6-dimethylpyrimidin-4-yl)-4-piperidylmethyl]piperazine a white solid/foam, 0.39 g (80%), mp73-74° C.;

Provenance & Evidence