Reaktion #94442

ord-e6a628c77d5e4abbaff5f78e9eabc531

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto the solution of the crude base in isopropanol, evaporation of this solution
  2. 2
    Sonstigein the rotary evaporator and recrystallisation of the residue from ethyl acetate

Vorschrift

Crude 2-[2-(N-methylcyclohexylamino)-phenylethenyl]-1-pyrroline is produced by heating the solution of 9.1 g (0.03 mole) of 2-(2-ethoxy-2-phenyl-ethenyl)-1-pyrroline-tetrafluoroborate in 20 ml of N-methyl-cyclohexylamine for 2 hours at 100°, and processing the reaction mixture analogously to Example 1. By addition of 2.8 g of methanesulphonic acid to the solution of the crude base in isopropanol, evaporation of this solution in the rotary evaporator and recrystallisation of the residue from ethyl acetate, there is obtained 2-[2-(N-methyl-cyclohexylamino)-phenylethenyl]-1-pyrroline-(1:1)-methanesulphonate, m.p. 163°-164°.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04130652uspto-grants-1978_12