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

HRID 324730
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 324730
[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-a689a3f577854ad0adf11e2116d74f2c
Quelldatensatz
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06218547B1

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