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Hydrochloric Acid → HCID 2836736, Verbindung

HRID 1012302
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1012302
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[C:15]([NH2:19])([CH3:18])([CH3:17])[CH3:16].Cl>C(Cl)(Cl)Cl>[C:15]([NH:19][S:8]([C:5]1[CH:6]=[CH:7][C:2]([CH3:1])=[C:3]([N+:12]([O-:14])=[O:13])[CH:4]=1)(=[O:10])=[O:9])([CH3:18])([CH3:17])[CH3:16]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 6385Tert-ButylamineHCID 5606384-Methyl-3-nitrobenzenesulfonyl chloride

Produkt 1

HCID 2836736HCID 2836736, VerbindungAusbeute 94,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To a solution of 4-methyl-3-nitrobenzenesulfonyl chloride (5.40 g, 22.9 mmol) in chloroform (50 ml) was added tert-butylamine (6.00 ml, 57.1 mmol) under ice-cooling, and the mixture was stirred at room temperature for 2.5 hr. To the reaction mixture was added 1N hydrochloric acid, and the mixture was extracted with chloroform. The organic layer was successively washed with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under reduced pressure, and hexane was added to the residue. The precipitated solid was collected by filtration and dried in vacuo to give N-tert-butyl-4-methyl-3-nitrobenzenesulfonamide (5.89 g, yield 94.6%).

Aufarbeitung

  1. temperaturecooling
  2. extractionthe mixture was extracted with chloroform
  3. washThe organic layer was successively washed with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationAfter filtration
  6. customthe solvent was evaporated under reduced pressure, and hexane
  7. additionwas added to the residue
  8. filtrationThe precipitated solid was collected by filtration
  9. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-0768500b70a1478b9785b10d729717e9
Quelldatensatz
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07977331B1

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