2-Chloro-3-nitropyridine → 2-Isothiocyanato-3-nitropyridine

HRID 6215

Reaktionsgleichung

Reaktionsgleichung von HRID 6215
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[N-:11]=[C:12]=[S:13].[K+]>C(O)(=O)C>[N:11]([C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1)=[C:12]=[S:13]

Komponenten

4

Edukt 2

HCID 796132-Chloro-3-nitropyridineHCID 10931372Isothiocyanatopotassium

Produkt 1

HCID 190433452-Isothiocyanato-3-nitropyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A 10 g sample of 2-chloro-3-nitropyridine, an 8 g sample of potassium isothiocyanate, and 75 ml of acetic acid were combined and refluxed for 2 h. The reaction mixture was then cooled and poured into 400 ml of ice/H2O. The resulting solid was washed with water, redissolved in ethyl acetate and washed (4×) with water. The ethyl acetate solution was then treated with activated carbon, dried over anhydrous Na2SO4, filtered and evaporated to dryness to provide 3.72 g of the title compound. m.p.=115°-118° C.

Aufarbeitung

  1. temperaturerefluxed for 2 h
  2. temperatureThe reaction mixture was then cooled
  3. washThe resulting solid was washed with water
  4. dissolutionredissolved in ethyl acetate
  5. washwashed (4×) with water
  6. additionThe ethyl acetate solution was then treated with activated carbon
  7. dry with materialdried over anhydrous Na2SO4
  8. filtrationfiltered
  9. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-f8af3a28440c4b40b27400296150885d
Quelldatensatz
uspto-grants-1993_09
Patentnummer
US05247073

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