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Dimethylamine → HCID 59896602, Verbindung

HRID 1457906
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1457906
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][NH:7][C:8](SC)=[CH:9][N+:10]([O-:12])=[O:11])=[CH:4][CH:3]=1.[CH3:17][NH:18][CH3:19]>CCO>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][NH:7][C:8]([N:18]([CH3:19])[CH3:17])=[CH:9][N+:10]([O-:12])=[O:11])=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 674DimethylamineHCID 70157188HCID 70157188, Verbindung

Produkt 1

HCID 59896602HCID 59896602, VerbindungAusbeute 47,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

In 100 ml of EtOH was dissolved 2.59 g (0.01 mole) of 1-(4-chlorobenzyl)amino-1-methylthio-2-nitroethylene with heating. Then, with refluxing and stirring, a solution of 2.25 g of 50% aqueous dimethylamine solution in 10 ml of EtOH was added dropwise over a period of 35 minutes. After completion of dropwise addition, the mixture was further stirred and refluxed for 2.5 hours. The solvent was then distilled off and the residue was diluted with ether and triturated, whereupon crystals separated. After addition of EtOH and ether (about 1:5), the crystals were collected by filtration, washed with ether and dried. The procedure gave 1.21 g of the title compound as white crystals.

Aufarbeitung

  1. temperaturewith heating
  2. temperatureThen, with refluxing
  3. additionAfter completion of dropwise addition
  4. stirringthe mixture was further stirred
  5. temperaturerefluxed for 2.5 hours
  6. distillationThe solvent was then distilled off
  7. additionthe residue was diluted with ether
  8. customtriturated, whereupon crystals
  9. customseparated
  10. additionAfter addition of EtOH and ether (about 1:5)
  11. filtrationthe crystals were collected by filtration
  12. washwashed with ether
  13. customdried

Quellen und Nachweise

ORD-Eintrag
ord-770de76926d44482a03fc36a390e4d81
Quelldatensatz
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05849768

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