Triethylamine → 2-Chloro-5-fluoropyridine-3-carbonitrile

HRID 510026Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 510026
C(N(CC)CC)C.[Cl:8][C:9]1[N:17]=[CH:16][C:15]([F:18])=[CH:14][C:10]=1[C:11]([NH2:13])=O.FC(F)(F)C(OC(=O)C(F)(F)F)=O>ClCCl>[Cl:8][C:9]1[N:17]=[CH:16][C:15]([F:18])=[CH:14][C:10]=1[C:11]#[N:13]

Komponenten

5

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

81.2 ml (582.25 mmol) of triethylamine were added to a suspension of 46.2 g (264.66 mmol) of 2-chloro-5-fluoronicotinamide in dichloromethane (783 ml), and the mixture was cooled to 0° C. Then, while stirring, 41.12 ml (291.13 mmol) of trifluoroacetic anhydride were slowly added dropwise and the mixture was stirred at 0° C. for 1.5 h. The reaction solution was subsequently washed twice with saturated aqueous sodium hydrogencarbonate solution (391 ml each time), dried and concentrated under reduced pressure.

Aufarbeitung

  1. stirringthe mixture was stirred at 0° C. for 1.5 h
  2. washThe reaction solution was subsequently washed twice with saturated aqueous sodium hydrogencarbonate solution (391 ml each time)
  3. customdried
  4. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-1389f5bc688941218dd67aeb143edb2c
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09096592B2

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