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Potassium Iodide → N-(4-(1-(4-(4-fluorophenyl)piperazin-1-yl)-1-methylethyl)phenylmethyl)acetamide dihydrochloride monohydrate

HRID 1282124
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1282124
[NH2:1][C:2]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][NH:12][C:13](=[O:15])[CH3:14])=[CH:7][CH:6]=1)([CH3:4])[CH3:3].[Cl:16][CH2:17][CH2:18][N:19]([CH2:27][CH2:28]Cl)[C:20]1[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CS(C)=O.O>[OH2:15].[ClH:16].[ClH:16].[F:26][C:23]1[CH:24]=[CH:25][C:20]([N:19]2[CH2:27][CH2:28][N:1]([C:2]([C:5]3[CH:10]=[CH:9][C:8]([CH2:11][NH:12][C:13](=[O:15])[CH3:14])=[CH:7][CH:6]=3)([CH3:3])[CH3:4])[CH2:17][CH2:18]2)=[CH:21][CH:22]=1
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Komponenten

7

Edukt 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 30941Aniline, N,N-bis(2-chloroethyl)-p-fluoro-HCID 18423109N-(4-(1-amino-1-methylethyl)phenylmethyl)acetamide

Produkt 1

HCID 18423145N-(4-(1-(4-(4-fluorophenyl)piperazin-1-yl)-1-methylethyl)phenylmethyl)acetamide dihydrochloride monohydrateAusbeute 22,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a solution of N-(4-(1-amino-1-methylethyl)phenylmethyl)-acetamide (1.55 g) and N,N-di(2-chloroethyl)-4-fluoroaniline (1.5 g) in dimethyl sulfoxide (30 ml) were added potassium carbonate (3.12 g) and potassium iodide (2.50 g) and the mixture was stirred at 80° C. for 24 hr. The reaction mixture was poured into water (300 ml) and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained residue was purified by silica gel chromatography (developing solvent; ethyl acetate:hexane=3:1) and treated with 1M hydrochloric acid-ether in ethanol to give the title compound (0.33 g) as white crystals.

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated
  5. customthe obtained residue was purified by silica gel chromatography (developing solvent; ethyl acetate:hexane=3:1)
  6. additiontreated with 1M hydrochloric acid-ether in ethanol

Quellen und Nachweise

ORD-Eintrag
ord-e5489caa0e9b47868fbcc60aa2f95bca
Quelldatensatz
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06455528B1

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