Reaktion #40944

ord-baa49772bb874fcea3044e6892cedd97

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenthe solution washed with aqueous saturated Na2S2O3 (3 mL) and NaHCO3 (3 mL)
  2. 2
    TrocknenThe organic phase was dried (Na2SO4)
  3. 3
    Sonstigeevaporated

Vorschrift

1-(4-Hydroxy-butyl)-5-(3-methyl-thiophen-2-yl)-1H-pyrimidine-2,4-dione (Prep 31, 30 mg, 0.11 mmol) was dissolved in dry DCM (2 mL), the solution was cooled to 0° C. and Dess-Martin periodinane (113 mg, 0.26 mmol) was added portionwise under nitrogen. The mixture was stirred at room temperature for 1.5 hours. Ethyl acetate was added and the solution washed with aqueous saturated Na2S2O3 (3 mL) and NaHCO3 (3 mL). The organic phase was dried (Na2SO4) and evaporated to give 30 mg of the title compound that was used in the next step without further purification (98% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07727988B2uspto-grants-2010_06