Diethylamine → 2-Chloro-N,N-diethylnicotinamide

HRID 1801493

Reaktionsgleichung

Reaktionsgleichung von HRID 1801493
[Cl:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[CH2:11]([NH:13][CH2:14][CH3:15])[CH3:12]>ClCCl>[Cl:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([N:13]([CH2:14][CH3:15])[CH2:11][CH3:12])=[O:5]

Komponenten

4

Edukt 2

HCID 8021DiethylamineHCID 27745412-Chloronicotinoyl chloride

Produkt 1

HCID 44659442-Chloro-N,N-diethylnicotinamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 2-chloronicotinoyl chloride (20.0 g, 114.3 mmol) in dichloromethane (100 mL) at 0° C. was added diethylamine (23.7 mL, 228.6 mmol). The reaction mixture was stirred overnight at room temperature, washed with water (3×100 mL), dried over sodium sulfate and concentrated under reduced pressure to provide the desired product as a brown oil. LC MS: 213 [M+H]. The crude product was used in Step 2 without any further purification.

Aufarbeitung

  1. washwashed with water (3×100 mL)
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7f887e8b1a2647beba2c6d228f3f17eb
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08349827B2

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