Réaction #93586

ord-f7b0d798c79c4e5d88ee89341c0c7a36

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreThe resulting solid was collected
  2. 2
    Lavagewashed thoroughly with ether-isopropanol (1:1, 50 mL)
  3. 3
    Autredried in vacuo at 50° C.

Mode opératoire

The free base, 3-[4-(3,4-dimethoxyphenyl)-4-isopropyl-4-cyanobutyl]-6,7-dimethoxy-N-methyl-1,2,3,4-tetrahydroisoquinoline (1, 15 g, 0.032 mol) was dissolved in isopropanol (70 mL) at 70° C., and 6M HCl in isopropanol (5.6 mL) slowly added. After cooling to room temperature, ether (40 mL) was added until the solution became cloudy (saturated), and the resulting mixture stirred overnight. The resulting solid was collected, washed thoroughly with ether-isopropanol (1:1, 50 mL), and dried in vacuo at 50° C. to yield 3-[4-(3,4-dimethoxyphenyl)-4-isopropyl-4-cyanobutyl]-6,7-dimethoxy-N-methyl-1,2,3,4-tetrahydroisoquinoline·HCl (1·HCl, 13.7 g, m.p. 115°-120° C.) as a white powder.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US04613606uspto-grants-1986_09