Réaction #505045

ord-bc2d2ada98c544b8a001f71f94e431e4

Conditions de réaction

Température
70°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurewas heated to 80 C for 4.5 h
  2. 2
    Extractionthe mixture was extracted with DCM (3×40 mL)
  3. 3
    Concentrationconcentrated

Mode opératoire

A mixture of but-3-ynyl 4-methylbenzenesulfonate (972 mg) and N-methyl piperazine (482 μL) was heated to 80 C for 4.5 h, diluted with 1,2-dichloroethane (5 mL) and heated to 70° C. for 18 h. Saturated aq. NaHCO3 was added (10 mL) and the mixture was extracted with DCM (3×40 mL), and concentrated to afford 0.70 g of 1-(but-3-ynyl)-4-methylpiperazine as a 3:2 mixture of tosylate salt and free base.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08093229B2uspto-grants-2012_01