Reacción #72693

ord-0be25a15013c4cb8b8bae2691e2304e5

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe reaction mixture was then partitioned between dichloromethane and saturated sodium bicarbonate (NaHCO3)
  2. 2
    LavadoThe organic layer was washed again with saturated NaHCO3
  3. 3
    Secadodried over sodium sulfate
  4. 4
    Concentraciónconcentrated to dryness in vacuo
  5. 5
    OtroThe residue was purified by preparative thin layer chromatography (PTLC) (silica; 4% methanol in dichloromethane)

Procedimiento

To a stirred solution of the product from Method C (0.03 grams, 0.114 mmol) dissolved in 5 mL of 10:1 dichloromethane/pyridine was added (0.018 grams, 0.228 mmol) of acetylchloride and the resulting mixture stirred at room temperature for 18 hours. The reaction mixture was then partitioned between dichloromethane and saturated sodium bicarbonate (NaHCO3). The organic layer was washed again with saturated NaHCO3, dried over sodium sulfate and concentrated to dryness in vacuo. The residue was purified by preparative thin layer chromatography (PTLC) (silica; 4% methanol in dichloromethane) affording 0.005 mg (15%) of the title compound as a colorless oil. LRMS: 288.1 (M+1).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08541426B2uspto-grants-2013_09