Reaktion #170255

ord-ad9462dac0964153bcf443371ef3345c

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGthe reaction mixture was stirred for a second time under microwave irradiations (100 W) at 80° C. for 30 minutes
  2. 2
    EinengenAfter concentration to dryness
  3. 3
    Sonstigethe residue was purified by chromatography on silica gel

Vorschrift

Potassium hydroxide (141 mg, 2.52 mmol) and thiophene-2-thiol (292 mg, 238 μL) were added to a solution of 1-benzhydrylazetidin-3-yl methanesulfonate (400 mg, 1.26 mmol) solubilized in THF (7 mL). The reaction mixture was stirred a first time under microwave irradiations (100 W) at 80° C. for 30 minutes. Potassium hydroxide (141 mg, 2.52 mmol) and thiophene-2-thiol (292 mg, 238 μL) were added and the reaction mixture was stirred for a second time under microwave irradiations (100 W) at 80° C. for 30 minutes. After concentration to dryness, the residue was purified by chromatography on silica gel using petroleum ether/ethyl acetate (1:0 to 9:1) as eluent. The title product was obtained as a yellow solid (160 mg, 37%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846711B2uspto-grants-2014_09