Réaction #63522

ord-927e402d66544e428ea75208f97b14a0

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températuremaintained under nitrogen
  2. 2
    Températureheated to 120° for 18 hr
  3. 3
    Autreafter which time a white solid had precipitated
  4. 4
    TempératureThe mixture was cooled
  5. 5
    Filtration, and the solid collected by filtration
  6. 6
    LavageThe solid was washed three times with isopropanol and vacuum
  7. 7
    Autredried at 100° for 48 hr

Mode opératoire

N-(4-Aminophenethyl)-1,2,3,4-tetrahydro-6,7-dimethoxy-1-methylisoquinoline dihydrochloride (10.0 g, 0.025 m) was dissolved in 49% HBr (25 ml) maintained under nitrogen and heated to 120° for 18 hr. after which time a white solid had precipitated. The mixture was cooled and the solid slurried with isopropanol (50 ml), stirred for 1 hr., and the solid collected by filtration. The solid was washed three times with isopropanol and vacuum dried at 100° for 48 hr. to give 8.5 g N-(4-aminophenethyl)-1,2,3,4-tetrahydro-6,7-dihydroxy-1-methylisoquinoline dihydrobromide as an off-white solid, m.p. 275°-278°.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US04766131uspto-grants-1988_08