Triethylamine → HCID 19989877, Verbindung

HRID 973424

Reaktionsgleichung

Reaktionsgleichung von HRID 973424
Cl[CH2:2][CH2:3][CH:4]1[C:9]2=[N:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N:8]2[C:7](=[O:17])[N:6]([CH3:18])[CH2:5]1.[N:19]1[CH:24]=[CH:23][CH:22]=[N:21][C:20]=1[N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH3:18][N:6]1[CH2:5][CH:4]([CH2:3][CH2:2][N:28]2[CH2:29][CH2:30][N:25]([C:20]3[N:19]=[CH:24][CH:23]=[CH:22][N:21]=3)[CH2:26][CH2:27]2)[C:9]2=[N:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N:8]2[C:7]1=[O:17]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 887471-(2-Pyrimidinyl)piperazineHCID 199898454-(2-Chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one

Produkt 1

HCID 19989877HCID 19989877, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To 60 mL of toluene was added 4.0 g (0.0152 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one, 6.0 g (0.033 mol) of 1-(2-pyrimidyl)piperazine, and 4.0 g (0.04 mol) of triethylamine. The reaction mixture was heated at reflux for 2 days and subsequently washed with 2×50 mL of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation. Crystallization from ethyl acetate afforded 4.0 g, 67% of analytically pure crystals, mp 161°-62° C.

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 2 days
  3. washsubsequently washed with 2×50 mL of 1N NaOH
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated by rotary evaporation
  7. customCrystallization from ethyl acetate
  8. customafforded 4.0 g, 67% of analytically pure crystals, mp 161°-62° C.

Quellen und Nachweise

ORD-Eintrag
ord-4468c9561fd34ace85f1afffbda719ff
Quelldatensatz
uspto-grants-1991_11
Patentnummer
US05063228

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