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Potassium Carbonate → HCID 14747672, Verbindung

HRID 483850
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 483850
[OH:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=[O:12])[CH:6]=[CH:5]2.C([O-])([O-])=O.[K+].[K+].[N:19]1([CH2:24][CH2:25][N:26]([CH2:34][CH:35]2[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]2)[C:27](=[O:33])[CH2:28][CH2:29][CH2:30][CH2:31]Cl)[CH2:23][CH2:22][CH2:21][CH2:20]1>CN(C)C=O>[N:19]1([CH2:24][CH2:25][N:26]([CH2:34][CH:35]2[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]2)[C:27]([CH2:28][CH2:29][CH2:30][CH2:31][O:1][C:2]2[CH:3]=[C:4]3[C:9](=[CH:10][CH:11]=2)[NH:8][C:7](=[O:12])[CH:6]=[CH:5]3)=[O:33])[CH2:23][CH2:22][CH2:21][CH2:20]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 1770652,6-DihydroxyquinolineHCID 20081659HCID 20081659, Verbindung

Produkt 1

HCID 14747672HCID 14747672, VerbindungAusbeute 10,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To 50 ml of dimethylformamide are added 1.73 g of 6-hydroxycarbostyril, 1.8 g of K2CO3 and 0.5 g of KI. To this mixture being stirred at 60°-70° C. is dropwise added 4.2 g of N-[2-(1-pyrrolidinyl)ethyl]-N-(5-chloropentanoyl)-cyclohexylmethylamine. Then, the mixture is stirred for 4 hours at the same temperature. The solvent is removed by evaporation. The residue is dissolved in 200 ml of chloroform and the solution is washed with diluted hydrochloric acid, a 1% aqueous sodium hydroxide solution and water in this order, and dried with anhydrous magnesium sulfate. The desiccant is removed by filtration and the filtrate is concentrated. The residue is purified by means of a silica gel column chromatography (eluent; chloroform:methanol=20:1) and recrystallized from diethyl ether to obtain 0.5 g of 6-[4-{N-[2-(1-pyrrolidinyl)ethyl]-N-cyclohexylmethylaminocarbonyl}-butoxy]carbostyril.

Aufarbeitung

  1. stirringThen, the mixture is stirred for 4 hours at the same temperature
  2. customThe solvent is removed by evaporation
  3. dissolutionThe residue is dissolved in 200 ml of chloroform
  4. washthe solution is washed with diluted hydrochloric acid
  5. dry with materiala 1% aqueous sodium hydroxide solution and water in this order, and dried with anhydrous magnesium sulfate
  6. customThe desiccant is removed by filtration
  7. concentrationthe filtrate is concentrated
  8. customThe residue is purified by means of a silica gel column chromatography (eluent; chloroform:methanol=20:1)
  9. customrecrystallized from diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-aee4692f01f74a16acc0ccb0d8268667
Quelldatensatz
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05227381

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