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Citric Acid → N-[[[N-(4-chloro-o-tolyl)-formimidoyl]methylamino]thio]-N-methyl-p-toluenesulfonamide

HRID 1648794
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1648794
[CH3:1][NH:2][S:3]([C:6]1[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][CH:7]=1)(=[O:5])=[O:4].C([N:15]([CH2:18]C)CC)C.[S:20](Cl)Cl.CN[CH:25]=[N:26][C:27]1[CH:32]=[C:31]([Cl:33])[CH:30]=[CH:29][C:28]=1[CH3:34].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>O.C(Cl)Cl>[Cl:33][C:31]1[CH:30]=[CH:29][C:28]([CH3:34])=[C:27]([N:26]=[CH:25][CH2:18][NH:15][S:20][N:2]([CH3:1])[S:3]([C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][CH:7]=2)(=[O:4])=[O:5])[CH:32]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 311Citric AcidHCID 8471Triethylamine2×HCID 12543N-Methyl-p-toluenesulfonamideHCID 25353Sulfur dichlorideHCID 178484923HCID 178484923, Verbindung

Produkt 1

HCID 86739104N-[[[N-(4-chloro-o-tolyl)-formimidoyl]methylamino]thio]-N-methyl-p-toluenesulfonamide
Ausbeute 8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a stirred solution cooled to -10° of 18.5 g. (0.1 mole) of N-methyl-p-toluenesulfonamide and 10.1 g. (0.1 mole) of triethylamine in 300 ml. of methylene chloride is added dropwise 10.3 g. (0.1 mole) sulfur dichloride. The reaction mixture is stirred at ambient temperature for 0.5 hour and cooled to 10°. A solution of 18.3 g (0.1 mole) of N-methyl-N'-(4-chloro-o-tolyl)formamidine and 10.1 g. (0.1 mole) triethylamine in 100 ml. of methylene chloride is added rapidly with stirring. The reaction mixture is stirred at ambient temperature for 0.5 hour and extracted successively with 300 ml. of water, 300 ml. aqueous citric acid solution containing 10.5 g. (0.05 mole) of citric acid, and 300 ml. of water. The organic layer is dried and the solvent removed under reduced pressure. The residue is chromatographed over 100 g. silica gel using Hexane:Et2O:Et3N (18:2:3 by volume) to obtain 3.2 g. (8% yield) of N-[[[N-(4-chloro-o-tolyl)-formimidoyl]methylamino]thio]-N-methyl-p-toluenesulfonamide as a viscous oil.

Aufarbeitung

  1. temperatureTo a stirred solution cooled to -10° of 18.5 g
  2. temperaturecooled to 10°
  3. stirringwith stirring
  4. stirringThe reaction mixture is stirred at ambient temperature for 0.5 hour
  5. extractionextracted successively with 300 ml
  6. additionaqueous citric acid solution containing 10.5 g
  7. customThe organic layer is dried
  8. customthe solvent removed under reduced pressure
  9. customThe residue is chromatographed over 100 g
  10. customto obtain 3.2 g

Quellen und Nachweise

ORD-Eintrag
ord-32b959f5850741daa9940681b2d38dea
Quelldatensatz
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04413013

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