Reacción #165927

ord-ed53fd13716f4c4797a5d3dd11b6677c

Disolventes

Condiciones de reacción

Temperatura
-2.5°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaby maintaining temp below 0° C
  2. 2
    OtroReaction mass
  3. 3
    OtroReaction mass
  4. 4
    Concentraciónwas concentrated to residue under vacuum at 40° C
  5. 5
    workup.DISSOLUTIONResidue was dissolved in Ethyl acetate (450 ml)
  6. 6
    Lavadowashed with sodium sulphite solution (10%, 2×135 ml)
  7. 7
    OtroReaction mass
  8. 8
    Concentraciónwas then concentrated to residue

Procedimiento

Ethyl-2-(4,5-dihydrofuran-3-yl)-2-oxoacetate (45 g) was dissolved in tetrahydrofuran (225 ml) and Methanol (45 ml). The reaction mass was cooled to −5 to 0° C. N-bromosuccinimide (47 g) was added lot wise by maintaining temp below 0° C. Reaction mass was then stirred at 20-25° C. for 12 hrs. Reaction mass was concentrated to residue under vacuum at 40° C. Residue was dissolved in Ethyl acetate (450 ml) and washed with sodium sulphite solution (10%, 2×135 ml). Reaction mass was then concentrated to residue to get ethyl-2-(3-bromo-2-methoxytetrahydrofuran-3-yl)-2-oxoacetate (Yield 63 g).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08841467B2uspto-grants-2014_09