Reaktionsgleichung
C(O[C:4]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[CH:5][C:6]1[CH2:10][CH2:9][CH2:8][N:7]=1)C.F[B-](F)(F)F.[CH3:22][S:23]([OH:26])(=[O:25])=[O:24].[CH3:27][NH:28][CH:29]1[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1>>[CH3:27][N:28]([CH:29]1[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1)[C:16]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH:4]=[CH:5][C:6]1[CH2:10][CH2:9][CH2:8][N:7]=1.[CH3:22][S:23]([O-:26])(=[O:25])=[O:24]Komponenten
5
Versuchsvorschrift
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°.
Aufarbeitung
- customto the solution of the crude base in isopropanol, evaporation of this solution
- customin the rotary evaporator and recrystallisation of the residue from ethyl acetate
Quellen und Nachweise
- ORD-Eintrag
- ord-e6a628c77d5e4abbaff5f78e9eabc531
- Quelldatensatz
- uspto-grants-1978_12
- Patentnummer
- US04130652
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