Dimethylformamide → 4-Dimethylamino-2-nitrobenzaldehyde

HRID 918553

Reaktionsgleichung

Reaktionsgleichung von HRID 918553
P(Cl)(Cl)(Cl)=O.[N+:6]([C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[N:12]([CH3:14])[CH3:13])([O-:8])=[O:7].CN(C)[CH:20]=[O:21]>>[N+:6]([C:9]1[CH:10]=[C:11]([N:12]([CH3:13])[CH3:14])[CH:15]=[CH:16][C:17]=1[CH:20]=[O:21])([O-:8])=[O:7]

Komponenten

4

Edukt 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 69269N,N-Dimethyl-3-nitroaniline

Produkt 1

HCID 2913524-Dimethylamino-2-nitrobenzaldehydeAusbeute 66 %

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

720 parts of phosphorus oxychloride is added at 25°C to a solution of 498 parts of m-nitrodimethylaniline in 1800 parts by volume of dimethylformamide. The mixture is then heated within 1 hour to 75° to 80°C and stirred at this temperature for six hours. After the solution has cooled it is poured into 6000 parts of ice-water. The precipitate is suction filtered, washed and recrystallized from acetone. 385 parts (66% of theory) of 2-nitro-4-dimethylaminobenzaldehyde having a melting point of 115° to 116°C is obtained. ##SPC14##

Aufarbeitung

  1. temperatureAfter the solution has cooled it
  2. filtrationfiltered
  3. washwashed
  4. customrecrystallized from acetone

Quellen und Nachweise

ORD-Eintrag
ord-d34ef8ca76e045609c7476aab3f3ae63
Quelldatensatz
uspto-grants-1976_07
Patentnummer
US03971821

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