Reaktion #85721

ord-fbe6f3c8987446e6bf8dd9e5b09fc317

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated
  2. 2
    workup.ADDITIONDCM (20 mL) and saturated NaHCO3 solution (10 mL) was added to the residue
  3. 3
    workup.STIRRINGThe mixture was stirred for 10 minutes
  4. 4
    Sonstigephases were separated
  5. 5
    ExtraktionAqueous layer was then extracted with DCM (2×10 mL)
  6. 6
    Trocknenthe combined organic was dried (Na2SO4)
  7. 7
    Einengenconcentrated

Vorschrift

To a solution of (R)—N—((R)-1-(1-(4-chlorophenyl)-1H-pyrazol-3-yl)ethyl)-2-methylpropane-2-sulfinamide (0.98 g, 3.01 mmol) in dioxane (10 ml) was added dropwise HCl (1.504 ml, 6.01 mmol). The reaction was stirred at room temperature for 30 minutes. LCMS indicated complete conversion to product. The reaction mixture was concentrated and DCM (20 mL) and saturated NaHCO3 solution (10 mL) was added to the residue. The mixture was stirred for 10 minutes and phases were separated. Aqueous layer was then extracted with DCM (2×10 mL), and the combined organic was dried (Na2SO4) and concentrated to give product (0.556 g). LCMS (B) m/z 222.2 (M+H)+

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434719B2uspto-grants-2016_09