Réaction #505462

ord-54f706a22a2144fd9d97ce541b5e2567

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrethe layers were separated
  2. 2
    Lavagethe organic layer was then washed with 2M NaOH solution (75 ml)
  3. 3
    Autrethe organic layers were separated
  4. 4
    Séchagedried (MgSO4)
  5. 5
    Concentrationconcentrated to dryness

Mode opératoire

To a solution of 1,1-dimethylethyl(3R)-3-methyl-1-piperazinecarboxylate (605 mg, 2.56 mmol) in DCM (20 ml) was added DIPEA (1.12 ml, 6.39 mmol) and then portionwise 4-[(trifluoromethyl)oxy]benzenesulfonyl chloride (0.455 ml, 2.68 mmol) at room temp and the resultant mixture stirred under Ar for 16 h. DCM (75 ml) and a 1M HCl solution (75 ml) were added, the layers were separated and the organic layer was then washed with 2M NaOH solution (75 ml), the organic layers were separated, dried (MgSO4) and concentrated to dryness. 1,1-Dimethylethyl(3R)-3-methyl-4-({4-[(trifluoromethyl)oxy]phenyl}sulfonyl)-1-piperazinecarboxylate was isolated as a slowly crystallizing white solid.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08093249B2uspto-grants-2012_01