Reacción #459149

ord-9b102aecb9524ba68ab1f2df0d4ed657

Disolventes

Condiciones de reacción

Temperatura
10°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    Otroto rise to 23° C
  3. 3
    Otrothe benzene layer separated
  4. 4
    Lavadowashed with 30 ml
  5. 5
    Secadowater, dried over anhydrous sodium sulfate
  6. 6
    Filtraciónfiltered
  7. 7
    Otro(93% yield) resulted

Procedimiento

To a solution of 0.48 g. (.012 m) of sodium hydroxide and 0.40 g. (.006 m) of 50% hydrogen peroxide in 10 ml. water at 10° C was added a solution of 2.7 g. (.0118 m) of 4-t-butylazo-4-cyanovaleryl chloride in 10 ml. benzene over 5 minutes. After the addition was complete, the reaction was stirred an additional 1/2 hour at 10° C and 15 minutes more allowing the temperature to rise to 23° C. Another 10 ml. benzene was added, the benzene layer separated, washed with 30 ml. 10% NaHCO3 solution, 15 ml. water, dried over anhydrous sodium sulfate, filtered and the benzene stripped off. A white crystalline solid weighing 2.3 g. (93% yield) resulted.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04088642uspto-grants-1978_05