Reaktion #79457

ord-3c7c6ddba54a4a5b969f9e051c8470aa

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    ExtraktionThe solution was extracted with ethyl acetate (10×25 ml)
  2. 2
    ExtraktionThe organic phase was extracted with saturated aqueous sodium chloride
  3. 3
    Trocknendried over magnesium sulfate
  4. 4
    Sonstigeevaporated to dryness, in vacuo

Vorschrift

3-(1-Thyminyl)-propanoic acid methyl ester (1.0 g, 0.0047 mol) was suspended in 2 M sodium hydroxide (15 ml), boiled for 10 min. The pH was adjusted to 0.3 with conc. hydrochloric acid. The solution was extracted with ethyl acetate (10×25 ml). The organic phase was extracted with saturated aqueous sodium chloride, dried over magnesium sulfate, and evaporated to dryness, in vacuo, to give the title compound as a white solid (0.66 g, 71%). M.p. 118-121° C. Anal. for C8H10N2O4, found (calc.) C, 48.38; (48.49); H, 5.09; (5.09); N, 13.93; (14.14). The compound showed satisfactory 1H and 13C-NMR spectra.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06713602B1uspto-grants-2004_03