Reacción #78361

ord-9e163ff779d74aa6810f4c0b5e5babcf

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturarefluxed for 10 minutes
  2. 2
    ExtracciónThe solution was extracted with ethyl acetate (10×25 mL)
  3. 3
    ExtracciónThe organic phase was extracted with saturated aqueous sodium chloride
  4. 4
    Secadodried over magnesium sulfate
  5. 5
    Otroevaporated to dryness in vacuo

Procedimiento

3-(1-Thyminyl)propanoic acid methyl ester (1 g, 0.0047 mol) was suspended in 2 M sodium hydroxide (15 mL), refluxed for 10 minutes. 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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06710164B1uspto-grants-2004_03