Potassium Carbonate → 2-Methyl-1-[4-(4-methylpiperazino)phenyl]-2-(4-methylpiperazino)-propan-1-one

HRID 981752Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 981752
F[C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:19])[C:9]([CH3:18])([N:11]2[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]2)[CH3:10])=[CH:4][CH:3]=1.[CH3:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1.C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[CH3:10][C:9]([N:11]1[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]1)([CH3:18])[C:8]([C:5]1[CH:6]=[CH:7][C:2]([N:24]2[CH2:25][CH2:26][N:21]([CH3:20])[CH2:22][CH2:23]2)=[CH:3][CH:4]=1)=[O:19]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 198794821-(4-Fluorophenyl)-2-methyl-2-(4-methylpiperazino)-propan-1-one

Produkt 1

HCID 198794312-Methyl-1-[4-(4-methylpiperazino)phenyl]-2-(4-methylpiperazino)-propan-1-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Reaktionsbedingungen

Temperatur
115 °C

Versuchsvorschrift

13.2 g (0.05 mol) of 1-(4-fluorophenyl)-2-methyl-2-(4-methylpiperazino)-propan-1-one and 6.5 g (0.065 mol) of 1-methylpiperazine are dissolved in 20 ml of dimethyl sulfoxide, and the solution is heated to about 115° C. together with 6.9 g (0.05 mol) of potassium carbonate. After 15 hours of stirring at about 115° C. the suspension is cooled down and is poured at about 60° C. onto ice. The crystals are filtered off and are recrystallised twice from ethyl acetate. Melting point 133°-136° C.

Aufarbeitung

  1. temperatureis cooled down
  2. additionis poured at about 60° C. onto ice
  3. filtrationThe crystals are filtered off
  4. customare recrystallised twice from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-0f21081b62ee42098af4acd170405558
Quelldatensatz
uspto-grants-1991_02
Patentnummer
US04992547

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