StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Dimethyl Sulfate → 1-Methyl-3-(3-nitrophenyl)pyridinium methyl sulfate

HRID 49813
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 49813
[N+:1]([C:4]1[CH:5]=[C:6]([C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[S:16]([O:21]C)([O:19][CH3:20])(=[O:18])=[O:17]>C(OCC)C>[CH3:20][O:19][S:16]([O-:21])(=[O:18])=[O:17].[CH3:20][N+:12]1[CH:13]=[CH:14][CH:15]=[C:10]([C:6]2[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)[CH:11]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6497Dimethyl Sulfate2×HCID 121813273-(3-Nitrophenyl)pyridine

Produkt 1

HCID 227418351-Methyl-3-(3-nitrophenyl)pyridinium methyl sulfateAusbeute 82 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

3-(3-nitrophenyl)pyridine (50 g, 0.25 mol) was added portion-wise with stirring to dimethyl sulfate (125 ml). The mixture was stirred at ambient temperature for 24 hours, during which time additional dimethyl sulfate was added (2×50 ml). At the end of the reaction diethyl ether (400 ml) was added, and the mixture was stirred in the cold for 2 hours. The precipitate was filtered off and washed several times with diethyl ether. Finally, the precipitate was stirred in pyridine (100 ml) at 45° C. for 30 min. THF (250 ml) was added. Stirring was continued for additionally 30 min whereafter the product was filtered off, washed with diethyl ether and dried to yield 1-methyl-3-(3-nitrophenyl)pyridinium methyl sulfate (66.6 g, 82%).

Aufarbeitung

  1. additionwas added (2×50 ml)
  2. additionwas added
  3. filtrationThe precipitate was filtered off
  4. washwashed several times with diethyl ether
  5. stirringFinally, the precipitate was stirred in pyridine (100 ml) at 45° C. for 30 min
  6. additionTHF (250 ml) was added
  7. stirringStirring
  8. waitwas continued for additionally 30 min whereafter the product
  9. filtrationwas filtered off
  10. washwashed with diethyl ether
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-882fde17102740048fe6d4b5925eed88
Quelldatensatz
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06710044B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion