Reaktion #62343

ord-4591426222324116a52532a1d4076497

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    workup.STIRRINGthe solution was stirred for 2 hours
  2. 2
    SonstigeThe diiodomethane was evaporated
  3. 3
    Sonstigethe crude product was purified
  4. 4
    Sonstigeseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:20)

Vorschrift

To a solution of 1.0 g of 2-amino-4-methyl-5-nitropyridine in 10 mL of diiodomethane was added 1.8 mL of isopentyl sulfite at room temperature, stirred at this temperature for 30 minutes, and after raising the temperature to 80° C., the solution was stirred for 2 hours. The diiodomethane was evaporated, and the crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:20), to afford 897 mg of the title compound as colorless crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07429609B2uspto-grants-2008_09