HCID 54250551, Verbindung → N-[2-[(3,4-Dichlorophenyl)sulfonyl]ethyl]-2-propanamine

HRID 745162Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 745162
C1(OC(=O)[N:9]([CH2:13][CH2:14][S:15]([C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[C:20]([Cl:25])[CH:19]=2)(=[O:17])=[O:16])[CH:10]([CH3:12])[CH3:11])C=CC=CC=1>Br>[Cl:25][C:20]1[CH:19]=[C:18]([S:15]([CH2:14][CH2:13][NH:9][CH:10]([CH3:12])[CH3:11])(=[O:16])=[O:17])[CH:23]=[CH:22][C:21]=1[Cl:24]

Komponenten

3

Edukt 1

HCID 54250551HCID 54250551, Verbindung

Produkt 1

HCID 14050280N-[2-[(3,4-Dichlorophenyl)sulfonyl]ethyl]-2-propanamineAusbeute 32,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 260Hydrogen BromideLösungsmittel

Versuchsvorschrift

A solution of 44.27 g (0.107 mole) of N-[2-[(3,4-dichlorophenyl)sulfonyl]ethyl]-N-(1-methylethyl)carbamic acid phenyl ester in 300 ml of 48% HBr was heated at reflux for 12 hr. The reaction mixture was cooled to room temperature, made alkaline with 50% sodium hydroxide-ice and extracted with chloroform. The chloroform layer was extracted with 1N sulfuric acid. The sulfuric acid layer was extracted with chloroform and the chloroform layers combined and evaporated to an oil, the free base of the title compound. A portion of the oil was reacted with ethereal hydrogen chloride to give an overall yield of 32.4% white crystaline product, m.p. 219°-221° C.

Aufarbeitung

  1. temperatureat reflux for 12 hr
  2. extractionextracted with chloroform
  3. extractionThe chloroform layer was extracted with 1N sulfuric acid
  4. extractionThe sulfuric acid layer was extracted with chloroform
  5. customevaporated to an oil
  6. customA portion of the oil was reacted with ethereal hydrogen chloride

Quellen und Nachweise

ORD-Eintrag
ord-5665680ad6fd4ce0aa03580362069ac6
Quelldatensatz
uspto-grants-1986_07
Patentnummer
US04597902

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