Formaldehyde → HCID 13115425, Verbindung

HRID 1075320Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1075320
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH3:11][C:12]([NH:14][C:15](C)=O)=[O:13].C=O>S(=O)(=O)(O)O>[CH3:10][C:7]1[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][C:6]=1[CH2:15][NH:14][C:12](=[O:13])[CH3:11]

Komponenten

5

Edukt 3

HCID 712FormaldehydeHCID 74734-NitrotolueneHCID 12263Diacetamide

Produkt 1

HCID 13115425HCID 13115425, VerbindungAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
55 °C

Versuchsvorschrift

To a solution of p-nitrotoluene (2.74 g; 0.02 mol) and diacetamide (4.24 g; 0.04 mol) in concentrated sulfuric acid (20 ml) is added aqueous formaldehyde (37%; 1.6 g; 0.02 mol) dropwise with stirring. The reaction mixture is stirred at room temperature for 17 hours, heated to 55° C. for 8 hours and then to 85° C. for 19 hours. The mixture is then poured onto ice. The resulting colorless precipitate is removed by filtration and recrystallized from aqueous ethanol to give 2.7 g of product (65% yield) having a melting point of 133° to 137.5° C.

Aufarbeitung

  1. stirringThe reaction mixture is stirred at room temperature for 17 hours
  2. additionThe mixture is then poured onto ice
  3. customThe resulting colorless precipitate is removed by filtration
  4. customrecrystallized from aqueous ethanol

Quellen und Nachweise

ORD-Eintrag
ord-e87131df6bfa48e1bf1bef72c29fee39
Quelldatensatz
uspto-grants-1983_07
Patentnummer
US04395577

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