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1,1-Dichloroethane → HCID 178526356, Verbindung

HRID 1836995
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1836995
ClC(Cl)C.[Cl:5][C:6]1[CH:7]=[C:8]([NH:12][C:13]([C:15]2[O:16][C:17]3[C:23]([N:24]4[CH2:28][CH2:27][CH2:26][CH2:25]4)=[CH:22][CH:21]=[CH:20][C:18]=3[CH:19]=2)=O)[CH:9]=[CH:10][CH:11]=1.P(Cl)(Cl)(Cl)(Cl)Cl.[ClH:35].[NH2:36][OH:37].C(N(CC)CC)C>C(#N)C.C(OCC)(=O)C>[Cl:35][C:19]1[C:18]2[CH:20]=[CH:21][CH:22]=[C:23]([N:24]3[CH2:28][CH2:27][CH2:26][CH2:25]3)[C:17]=2[O:16][C:15]=1[C:13]([NH:12][C:8]1[CH:9]=[CH:10][CH:11]=[C:6]([Cl:5])[CH:7]=1)=[N:36][OH:37]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 63651,1-DichloroethaneHCID 8471TriethylamineHCID 24819Phosphorus pentachlorideHCID 443297Hydroxyamine hydrochlorideHCID 12150613HCID 12150613, Verbindung

Produkt 1

HCID 178526356HCID 178526356, VerbindungAusbeute 13 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6342AcetonitrileLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
75 °C

Versuchsvorschrift

To a dichloroethane solution of 7-pyrrolidin-1-yl-benzofuran-2-carboxylic acid (3-chloro-phenyl)-amide (343 mg, 1 μM) was added phosphorous pentachloride (210 mg, 1.2 mmol), and the mixture was stirred at 75° C. for 2 hours. The solvent was removed under vacuum, the mixture was treated with 5 ml of toluene and then was evaporated to dryness under vacuum. The residue was dissolved in acetonitrile and was added to another flask containing 210 mg (3 mmol) hydroxylamine hydrochloride and triethyl amine 701 μL (5 mmol) in acetonitrile at 0° C. The mixture was allowed to stir overnight. The reaction mixture was diluted with ethyl acetate, washed with 1 N HCl (2×) and brine. The organic layer was dried over MgSO4, filtered and stripped. The crude product was purified by flash chromatography on silica gel eluted with hexane/ethyl acetate (20:1) to give 43 mg of 3-chloro-N-(3-chloro-phenyl)-N′-hydroxy-7-pyrrolidin-1-yl-benzofuran-2-carboxamidine in 13% yield.

Aufarbeitung

  1. customThe solvent was removed under vacuum
  2. additionthe mixture was treated with 5 ml of toluene
  3. customwas evaporated to dryness under vacuum
  4. dissolutionThe residue was dissolved in acetonitrile
  5. additionwas added to another flask
  6. stirringto stir overnight
  7. washwashed with 1 N HCl (2×) and brine
  8. dry with materialThe organic layer was dried over MgSO4
  9. filtrationfiltered
  10. customThe crude product was purified by flash chromatography on silica gel
  11. washeluted with hexane/ethyl acetate (20:1)

Quellen und Nachweise

ORD-Eintrag
ord-104e81506e3e4debb7248071e92fab2a
Quelldatensatz
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06780858B2

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