Iodine → 2-Iodo-6-(trifluoromethyl)pyridin-3-amine

HRID 12306

Reaktionsgleichung

Reaktionsgleichung von HRID 12306
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([F:11])([F:10])[F:9])=[N:6][CH:7]=1.[I:12]I>C(O)C.S([O-])([O-])(=O)=O.[Ag+2]>[NH2:1][C:2]1[C:7]([I:12])=[N:6][C:5]([C:8]([F:11])([F:9])[F:10])=[CH:4][CH:3]=1

Komponenten

5

Edukt 2

HCID 807IodineHCID 27377445-Amino-2-(trifluoromethyl)pyridine

Produkt 1

HCID 534254792-Iodo-6-(trifluoromethyl)pyridin-3-amineAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418844HCID 178418844, VerbindungKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

3.85 g (12.3 mM) of silver sulfate are added, with stirring and at room temperature, to a solution of 2 g (12.3 mM) of 5-amino-2-(trifluoromethyl)pyridine in 100 ml of ethanol. 3.13 g of iodine are then added and the reaction mixture is stirred at room temperature for 24 hours. The solid in suspension in the medium is removed by filtration and the filtrate is concentrated under reduced pressure. The evaporation residue is taken up in 200 ml of dichloromethane and washed with 5% sodium hydroxide solution, and then with water and dried over magnesium sulfate. The solution obtained is concentrated under reduced pressure and 3.42 g of the expected compound are thus obtained in the form of a pink solid (yield=96%).

Aufarbeitung

  1. customThe solid in suspension in the medium is removed by filtration
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. washwashed with 5% sodium hydroxide solution
  4. dry with materialwith water and dried over magnesium sulfate
  5. customThe solution obtained
  6. concentrationis concentrated under reduced pressure and 3.42 g of the expected compound

Quellen und Nachweise

ORD-Eintrag
ord-d8ab2f2da6704ce983b0aa772fa77a07
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07728002B2

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