Reacción #511797

ord-2746160143f3431d87b51cf99af4bdec

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawhile cooling with ice
  2. 2
    Extracciónextracted with diethyl ether (4×100 ml)
  3. 3
    SecadoThe organic phase was dried over sodium sulfate
  4. 4
    Concentraciónconcentrated i
  5. 5
    Otroand the product was obtained as a white solid

Procedimiento

40 percent strength aqueous dimethylamine solution (85 ml, 0.67 mol), 1,4-dioxa-spiro[4.5]decane-8-carbaldehyde (240 g, 0.141 mol) and potassium cyanide (22.05 g, 0.338 mol) were added to a mixture of 4 N hydrochloric acid (37 ml) and methanol (22 ml), while cooling with ice. The mixture was stirred at room temperature for 4 d and then, after addition of water (80 ml), extracted with diethyl ether (4×100 ml). The organic phase was dried over sodium sulfate and concentrated i. vac. and the product was obtained as a white solid. Yield: 25.2 g (81%), melting point: 48-51° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08106055B2uspto-grants-2012_01