Potassium Iodide → 1-{3-[4-[Bis(4-fluorophenyl)methylene]piperidino]propyl}-4-(2-pyrimidinyl)piperazine dihydrochloride

HRID 1460449Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1460449
[Cl:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][N:8]([C:11]2[N:16]=[CH:15][CH:14]=[CH:13][N:12]=2)[CH2:7][CH2:6]1.[F:17][C:18]1[CH:23]=[CH:22][C:21]([C:24]([C:31]2[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=2)=[C:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CC(C)CC(=O)C>[ClH:1].[ClH:1].[F:37][C:34]1[CH:35]=[CH:36][C:31]([C:24]([C:21]2[CH:20]=[CH:19][C:18]([F:17])=[CH:23][CH:22]=2)=[C:25]2[CH2:30][CH2:29][N:28]([CH2:2][CH2:3][CH2:4][N:5]3[CH2:10][CH2:9][N:8]([C:11]4[N:16]=[CH:15][CH:14]=[CH:13][N:12]=4)[CH2:7][CH2:6]3)[CH2:27][CH2:26]2)=[CH:32][CH:33]=1

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 27244364-(Bis(4-fluorophenyl)methylene)piperidineHCID 148827373-[4-(2-Pyrimidinyl)piperazinyl]propyl chloride

Produkt 1

HCID 199157831-{3-[4-[Bis(4-fluorophenyl)methylene]piperidino]propyl}-4-(2-pyrimidinyl)piperazine dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7909Methyl Isobutyl KetoneLösungsmittel

Versuchsvorschrift

A mixture of 0.89 g of 1-(3-chloropropyl)-4-(2-pyrimidinyl)piperazine, 0.80 g of 4-[bis(4-fluorophenyl)methylene]piperidine and 0.51 g of potassium carbonate in 30 ml of 4-methyl-2-pentanone is brought to reflux for 48 hours in the presence of a trace of potassium iodide. The solvent is evaporated off and the residue is taken up in dichloromethane. The solution is washed with water. It is concentrated. The residue obtained is purified on a silica column using a mixture of dichloromethane and methanol (80:20 V/V) as eluent.

Aufarbeitung

  1. customThe solvent is evaporated off
  2. washThe solution is washed with water
  3. concentrationIt is concentrated
  4. customThe residue obtained
  5. customis purified on a silica column
  6. additiona mixture of dichloromethane and methanol (80:20 V/V) as eluent

Quellen und Nachweise

ORD-Eintrag
ord-cdf4ecfb43b6478e81a937b37aff5d71
Quelldatensatz
uspto-grants-1991_12
Patentnummer
US05071847

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