Reaktionsgleichung
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl[CH2:10][CH2:11][CH:12]1[C:17]2=[N:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[N:16]2[C:15](=[O:25])[N:14]([CH3:26])[CH2:13]1>>[CH3:26][N:14]1[CH2:13][CH:12]([CH2:11][CH2:10][N:2]([CH3:1])[C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)[C:17]2=[N:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[N:16]2[C:15]1=[O:25]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 90 °C
Versuchsvorschrift
To 15 mL of N-methylaniline was added 3.5 g (0.0133 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one. The reaction mixture was heated to 90° C. (oil bath) for 2 days, and the excess N-methylaniline removed in vacuo at 80° C., 0.5 mm Hg. The residue was dissolved in 100 mL of CH2Cl2, washed with 2×100 mL of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation. The residue was subjected to high vacuum (0.5 mm, Hg) at 85° C. for 2 hr, and then crystallized from iso-octane/toluene to give 2.3 g (52%) of analytically pure crystals, mp 130°-31° C.
Aufarbeitung
- customthe excess N-methylaniline removed in vacuo at 80° C.
- dissolutionThe residue was dissolved in 100 mL of CH2Cl2
- washwashed with 2×100 mL of 1N NaOH
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated by rotary evaporation
- customcrystallized from iso-octane/toluene
- customto give 2.3 g (52%) of analytically pure crystals, mp 130°-31° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-c78e2a38ff4646a4a82c085bb73e74cf
- Quelldatensatz
- uspto-grants-1991_11
- Patentnummer
- US05063228
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