Reacción #2336532

ord-15dbeaa659714f6b84db64de5621342e

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Filtraciónthen filtered
  2. 2
    OtroThe filter cake was purified by flash column chromatography (gradient elution 10%-30% ethyl acetate:isohexane)

Procedimiento

Thiophenol (11.75 g, 107 mmol), potassium carbonate (14.74 g, 107 mmol) and ditosylated dicyanohydroquinone (25.00 g, 53.0 mmol) in DMF (80 mL) were reacted as described above. Water (100 mL) was added and the mixture stirred for 1 hour then filtered. The filter cake was purified by flash column chromatography (gradient elution 10%-30% ethyl acetate:isohexane) to give the title compound as a yellow solid (5.53 g, 16.1 mmol, 52%). [Found: C, 69.6%; H, 3.5%; N, 8.2%; S, 18.3%; C20H12N2S2 requires C, 69.8%; H, 3.5%; N, 8.1%; S, 18.6%]; MS (EI+) 344 (M+, 100%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07314511B2uspto-grants-2008_01