Pyridine → 6-Chloro-2-(ethylamino)pyridine-3-carbonyl fluoride

HRID 2207305Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2207305
N1C=CC=CC=1.[F:7]N1N=C(F)C=C(F)N1.[Cl:16][C:17]1[CH:25]=[CH:24][C:20]([C:21](O)=[O:22])=[C:19]([NH:26][CH2:27][CH3:28])[N:18]=1>ClCCl>[Cl:16][C:17]1[CH:25]=[CH:24][C:20]([C:21]([F:7])=[O:22])=[C:19]([NH:26][CH2:27][CH3:28])[N:18]=1

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 216944332,4,6-Trifluoro-1,2,3-triazineHCID 633764796-Chloro-2-(ethylamino)nicotinic acid

Produkt 1

HCID 867145746-Chloro-2-(ethylamino)pyridine-3-carbonyl fluorideAusbeute 99,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

2 ml (24.8 mmol) of pyridine and 4.2 ml (49.8 mmol) of 2,4,6-trifluorotriazine were added to a suspension of 5.0 g (24.8 mmol) of 6-chloro-2-ethylamino-nicotinic acid in 125 ml of dichloromethane. The mixture was stirred for 3 hours at ambient temperature and then filtered. The solid was rinsed with 50 ml of dichloromethane and the filtrate was washed twice with 60 ml of ice-cold water. The organic phase was dried over Na2SO4 and the solvent was evaporated off under reduced pressure. 5.01 g of product were obtained in the form of an orange oil which was used without further purification.

Aufarbeitung

  1. filtrationfiltered
  2. washThe solid was rinsed with 50 ml of dichloromethane
  3. washthe filtrate was washed twice with 60 ml of ice-cold water
  4. dry with materialThe organic phase was dried over Na2SO4
  5. customthe solvent was evaporated off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-892b107875144d8fb9d2bc4c30046293
Quelldatensatz
uspto-grants-2016_06
Patentnummer
US09376432B2

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