Reacción #409681

ord-933cdc11f8914b989e7d03b51e731aa8

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrofollowed by removal of the cooling bath
  2. 2
    workup.WAITAfter 1 h
  3. 3
    workup.ADDITIONthe reaction mixture was diluted with EtOAc
  4. 4
    Lavadowashed with H2O, sat. NaHCO3 and brine
  5. 5
    Secadodried (MgSO4)
  6. 6
    Concentraciónconcentrated

Procedimiento

To a rapidly stirred solution of 2-3 (0.86 g, 4.3 mmol) and THF (25 mL) at −78° C. was added NaN(TMS)2 (5.2 mL, 5.2 mmol, 1.0 M in THF). After 20 min, ethyl bromoacetate (0.58 mL, 5.2 mmol) was added followed by removal of the cooling bath. After 1 h, the reaction mixture was diluted with EtOAc and then washed with H2O, sat. NaHCO3 and brine, dried (MgSO4), and concentrated to give 2-4 as a yellow oil.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06211184B1uspto-grants-2001_04