Reacción #40668

ord-5b1739874cf74cd0a4adf4f3312b5832

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaat reflux for 2.5 h
  2. 2
    FiltraciónThe reaction mixture was filtered through a cake of Celite®
  3. 3
    Lavadowashed the cake with CH2Cl2
  4. 4
    OtroThe solvent was evaporated under reduced pressure
  5. 5
    OtroThe desired product was purified by column chromatography
  6. 6
    Otroover 60 min
  7. 7
    Lavadoas eluting gradient

Procedimiento

To a solution of 2e (40 mg, 0.168 mmol) in CH2Cl2 was added benzoyl isothiocyanate (30 mg, 0.189 mmol). The reaction mixture was kept at reflux for 2.5 h. The reaction mixture was filtered through a cake of Celite® and washed the cake with CH2Cl2. The solvent was evaporated under reduced pressure. The desired product was purified by column chromatography using 0 to 80% EtOAc in hexane over 60 min as eluting gradient to afford 2f (76 mg, 99%) as a powder. MS (ES) m/z 402 [M+H]+.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07728008B2uspto-grants-2010_06