5-Chloro-2-nitropyridine → 5-(Methylthio)-2-nitropyridine

HRID 917861Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 917861
Cl[C:2]1[CH:3]=[CH:4][C:5]([N+:8]([O-:10])=[O:9])=[N:6][CH:7]=1.[CH3:11][S-:12].[Na+]>C(O)C>[CH3:11][S:12][C:2]1[CH:3]=[CH:4][C:5]([N+:8]([O-:10])=[O:9])=[N:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 2598065-Chloro-2-nitropyridineHCID 4378561Sodium methanethiolate2×

Produkt 1

HCID 220361825-(Methylthio)-2-nitropyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

5-Chloro-2-nitropyridine (8.0 grams) was added to a solution of 2.5 grams of sodium methanethiolate in 100 milliliters of ethanol at a temperature of 0°C. to which solution excess sodium methanethiolate was added portionwise. The resulting reaction mixture was then heated to reflux and refluxed for 15 hours with constant stirring. At the end of the 15 hours, the reaction mixture was filtered and allowed to concentrate to 75 milliliters. The reaction mixture was then permitted to cool and filtered again, yielding the desired 5-(methylthio)-2-nitropyridine; it was recrystallized from ethanol, m.p., 100.5°-02.5°C.

Aufarbeitung

  1. additionwas added portionwise
  2. customThe resulting reaction mixture
  3. temperaturewas then heated
  4. temperatureto reflux
  5. temperaturerefluxed for 15 hours with constant stirring
  6. filtrationAt the end of the 15 hours, the reaction mixture was filtered
  7. concentrationto concentrate to 75 milliliters
  8. temperatureto cool
  9. filtrationfiltered again

Quellen und Nachweise

ORD-Eintrag
ord-d713405093b54466aed4a578972d3764
Quelldatensatz
uspto-grants-1976_07
Patentnummer
US03968116

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