Reacción #367328

ord-032e3c2be01c4129889814826fa7ebd1

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawhile maintaining a reaction temperature of ≤10° C
  2. 2
    Otrothe ice bath is removed
  3. 3
    Otroto reach RT
  4. 4
    FiltraciónThe solids are filtered
  5. 5
    Lavadowashed with dry toluene
  6. 6
    Otrothe filtrate evaporated in vacuo

Procedimiento

A solution of titanium tetrachloride (53.8 g, 31.2 ml) in dry toluene (200 ml) is added over a period of 45 minutes to a stirred solution of 7-methoxy-1-tetralone (100.5 g) and dimethyl amine (171 g) in dry toluene (2 l) while maintaining a reaction temperature of ≤10° C. When the addition of the titanium is complete, the ice bath is removed and the solution allowed to reach RT. The solution is stirred at RT for 3 hours. The solids are filtered, washed with dry toluene and the filtrate evaporated in vacuo, yielding 101.4 g of an amber oil which is used in the next step without further treatment.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04588719uspto-grants-1986_05