Ethylene Glycol → HCID 86643578, Verbindung

HRID 1848962Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1848962
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[C:5](I)=[CH:4][N:3]=1.[C:10]1([SH:16])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(O)CO.C(=O)([O-])[O-].[K+].[K+]>[Cu]I.C(O)(C)C>[Cl:1][C:2]1[C:7]([S:16][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=1

Komponenten

7

Edukt 4

HCID 174Ethylene GlycolHCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 454803662-Chloro-5-iodopyridin-4-amine

Produkt 1

HCID 86643578HCID 86643578, VerbindungAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)KatalysatorHCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

To a 250 mL round flask was added 2-chloro-5-iodo-4-aminopyridine (5.0 g, 19.6 mmol), thiophenol (2.16 g, 19.6 mmol), CuI (0.187 g, 0.98 mmol), ethylene glycol (2.5 g, 39 mmol), potassium carbonate (5.4 g, 39 mmol), and 150 mL of isopropanol. The reaction was heated to reflux and stirred under a nitrogen atmosphere for 24 h. After cooling, the mixture was purified by a silica gel column. Yield (97%) of 2-chloro-3-phenylthio-4-aminopyridine was 4.5 g.

Aufarbeitung

  1. temperatureThe reaction was heated
  2. temperatureto reflux
  3. temperatureAfter cooling
  4. customthe mixture was purified by a silica gel column

Quellen und Nachweise

ORD-Eintrag
ord-7bb80aa41eaf411fa931a8b21c79ebf4
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08952363B2

Notizen zur Reaktion

Wird geladen…