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Hydrochloric Acid → HCID 87462564, Verbindung

HRID 534693
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 534693
[C:1]1([S:7][C:8]([S:11](F)(=[O:13])=[O:12])([F:10])[F:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:15]([NH2:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.Cl>ClCCCl>[CH2:15]([NH:22][S:11]([C:8]([F:10])([F:9])[S:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)(=[O:13])=[O:12])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 7504BenzylamineHCID 23726265HCID 23726265, Verbindung2×

Produkt 1

HCID 87462564HCID 87462564, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Versuchsvorschrift

Added to a solution of 1,2-dichloroethane (15 ml), containing the PhSCF2SO2F (1.46 g, 5 mmol) obtained according to the method from example 7, was freshly distilled benzylamine (2.7 ml, 25 mmol). The mixture was stirred and heated at 50° C. for 20 h until the disappearance of PhSCF2SO2F (monitored by TLC and 19F NMR/CDCl3). After returning to ambient temperature, an aqueous solution of HCl (10%) was added to the reaction medium. The aqueous and organic phases were separated and the aqueous phase was extracted with dichloromethane. The organic phases were combined and dried over MgSO4. After filtration and evaporation of the solvents, the residue was purified by chromatography over silica gel (pentane to pentane/AcOEt:4/1). The sulfonamide product was obtained in the form of a white solid (1.5 g, 90%).

Aufarbeitung

  1. customobtained
  2. customAfter returning to ambient temperature
  3. customThe aqueous and organic phases were separated
  4. extractionthe aqueous phase was extracted with dichloromethane
  5. dry with materialdried over MgSO4
  6. filtrationAfter filtration and evaporation of the solvents
  7. customthe residue was purified by chromatography over silica gel (pentane to pentane/AcOEt:4/1)

Quellen und Nachweise

ORD-Eintrag
ord-33364c33f978447a95ccffb5ee2ccdd5
Quelldatensatz
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08853448B2

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