Iodine → HCID 178503563, Verbindung

HRID 1048754Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1048754
[I:1]I.[OH:3][C:4]1[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[C:6]([S:12][CH3:13])[N:5]=1>C(O)C.S([O-])([O-])(=O)=O.[Ag+2]>[OH:3][C:4]1[C:11]([I:1])=[CH:10][C:7]([C:8]#[N:9])=[C:6]([S:12][CH3:13])[N:5]=1

Komponenten

5

Edukt 2

HCID 807IodineHCID 178503531HCID 178503531, Verbindung

Produkt 1

HCID 178503563HCID 178503563, VerbindungAusbeute 90,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418844HCID 178418844, VerbindungKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

6 g (1.6 eq) of silver sulfate and 4.58 g (1.5 eq) of iodine are added successively to a solution of 2 g (12 mmol) of 6-hydroxy-2-(methylthio)nicotinonitrile in 200 ml of ethanol. The reaction medium is stirred at room temperature for 2 hours. The solid is filtered and the residue rinsed thoroughly with methanol. The filtrate is evaporated and then taken up in ethyl acetate. The organic phase is washed with water three times, dried on magnesium sulfate and evaporated to yield 3.18 g (90%) of 6-hydroxy-5-iodo-2-(methylthio)nicotinonitrile in the form of a yellow powder.

Aufarbeitung

  1. filtrationThe solid is filtered
  2. washthe residue rinsed thoroughly with methanol
  3. customThe filtrate is evaporated
  4. washThe organic phase is washed with water three times
  5. customdried on magnesium sulfate
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-57539934857c4e78a45be677c930a753
Quelldatensatz
uspto-grants-2016_07
Patentnummer
US09381195B2

Notizen zur Reaktion

Wird geladen…