Reacción #748648

ord-8990923d73b84037b6ceeb47438a817e

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturathe mixture was heated
  2. 2
    Temperaturato reflux for 2 hours
  3. 3
    Otrothe organic layer was separated
  4. 4
    Lavadowashed with water
  5. 5
    Secadoa saturated brine, dried over magnesium sulfate
  6. 6
    Concentraciónconcentrated in vacuo

Procedimiento

1M lithium tri-tert-butoxy-aluminohydride/tetrahydrofuran solution (14 ml) was added dropwise to a solution of tert-butyl methyl 2,2-dimethyl-malonate (1.12 g) in tetrahydrofuran (30 ml) under nitrogen atmosphere over 15 minutes and the mixture was heated to reflux for 2 hours. The reaction mixture was cooled to room temperature, a saturated ammonium chloride aq. solution and ethyl acetate were added and the organic layer was separated, washed with water and a saturated brine, dried over magnesium sulfate and concentrated in vacuo to give the titled compound (800 mg). MS (m/z): 175 [M+H]+.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08084611B2uspto-grants-2011_12