Water → HCID 86616333, Verbindung

HRID 499789Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 499789
[I:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]2=O)=[CH:4][CH:3]=1.C([O-])(O)=O.[Na+].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:21].O>O1CCOCC1.C(Cl)Cl>[I:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]2=[S:21])=[CH:4][CH:3]=1

Komponenten

7

Edukt 4

HCID 962WaterHCID 14817Phosphorus sulfide (P2S5)HCID 516892Sodium BicarbonateHCID 18453089HCID 18453089, Verbindung

Produkt 1

HCID 86616333HCID 86616333, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 1-(4-iodophenyl)pyridin-2(1H)-one prepared above (0.760 g, 2.56 mmol), NaHCO3 (2.15 g, 25.6 mmol) and P2S5 (2.27 g, 10.2 mmol) in dioxane (20 mL) was heated at 80° C. overnight. After being cooled to room temperature, water and CH2Cl2 were added. The organic layer was separated, washed with brine, dried over Na2SO4, concentrated in vacuo to give 1-(4-iodophenyl)pyridine-2(1H)-thione as a solid (0.752 g). MS 313.8 (M+H).

Aufarbeitung

  1. temperatureAfter being cooled to room temperature
  2. customThe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-b9119f876b594531bf41b61a2e8e450b
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07767697B2

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