Potassium Iodide → HCID 178432282, Verbindung

HRID 1089759Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1089759
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[C:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:4][CH:3]=1.[Cl:21][CH2:22][CH2:23][C:24]1[C:25]([CH3:36])=[N:26][C:27]2[N:28]([CH:31]=[N:32][C:33]=2[C:34]#[N:35])[C:29]=1[OH:30].C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>CC(C)CC(=O)C>[ClH:21].[C:34]([C:33]1[N:32]=[CH:31][N:28]2[C:29]([OH:30])=[C:24]([CH2:23][CH2:22][N:12]3[CH2:11][CH2:10][C:9](=[C:8]([C:5]4[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=4)[C:15]4[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=4)[CH2:14][CH2:13]3)[C:25]([CH3:36])=[N:26][C:27]=12)#[N:35]

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 150203584-[(4-Fluorophenyl)(phenyl)methylidene]piperidineHCID 178432280HCID 178432280, Verbindung

Produkt 1

HCID 178432282HCID 178432282, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7909Methyl Isobutyl KetoneLösungsmittel

Versuchsvorschrift

A mixture containing 0.0046 mol of 4-[(4-fluorophenyl)phenylmethylene]piperidine, 0.0055 mol of the compound obtained in Stage A, 0.028 mol of sodium carbonate and 0.1 g of potassium iodide in 100 ml of 4-methyl-2-pentanone is brought to reflux for 8 hours. The mixture is concentrated under vacuum. The residue is taken up in water and the product is extracted with dichloromethane. After evaporation of the solvent, the product is solubilized in a mixture of ethyl ether and acetone and converted to a hydrochloride after the addition of hydrochloric acid. The salt is recrystallized in acetone.

Aufarbeitung

  1. temperatureto reflux for 8 hours
  2. concentrationThe mixture is concentrated under vacuum
  3. extractionthe product is extracted with dichloromethane
  4. customAfter evaporation of the solvent
  5. additionthe product is solubilized in a mixture of ethyl ether and acetone
  6. additionafter the addition of hydrochloric acid
  7. customThe salt is recrystallized in acetone

Quellen und Nachweise

ORD-Eintrag
ord-a14223c12bdb4d0eb74cb0f7dcbb2e02
Quelldatensatz
uspto-grants-1992_01
Patentnummer
US05079249

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