Реакция #93586

ord-f7b0d798c79c4e5d88ee89341c0c7a36

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04613606uspto-grants-1986_09