Dimethylamine → 4-tert-Butyl-N,N-dimethyl-2,6-dinitroaniline

HRID 1678834Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1678834
[N+:1]([C:4]1[CH:9]=[C:8]([C:10]([CH3:13])([CH3:12])[CH3:11])[CH:7]=[C:6]([N+:14]([O-:16])=[O:15])[C:5]=1Cl)([O-:3])=[O:2].[CH3:18][NH:19][CH3:20].C(O)C>O>[CH3:18][N:19]([CH3:20])[C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:9][C:8]([C:10]([CH3:13])([CH3:12])[CH3:11])=[CH:7][C:6]=1[N+:14]([O-:16])=[O:15]

Komponenten

5

Edukt 3

HCID 674DimethylamineHCID 702EthanolHCID 751764-tert-Butyl-2,6-dinitrochlorobenzene

Produkt 1

HCID 203642434-tert-Butyl-N,N-dimethyl-2,6-dinitroaniline

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Two and six-tenths grams (.01 mole) of 2,6-dinitro-4-t-butylchlorobenzene was reacted with 3.1 grams of 40% aqueous solution of dimethylamine in 50 ml. ethanol. The temperature was slowly increased as follows: 30° C. for 1 hour, 40° C. for 1 hour, 50° C. for one hour, then 80° C. for five hours. When the reaction was complete, about 100 ml. H2O was added, precipitating the product. This was filtered, washed with portions of H2O and upon recrystallization from ethanol yielded 2.5 grams of N,N-dimethyl-2,6-dinitro-4-t-butylaniline in the form of orange-yellow needles melting at 101-102° C.

Aufarbeitung

  1. temperatureThe temperature was slowly increased
  2. wait40° C. for 1 hour
  3. wait50° C. for one hour
  4. wait80° C. for five hours
  5. customprecipitating the product
  6. filtrationThis was filtered
  7. washwashed with portions of H2O and upon recrystallization from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-3e70a35179374916b3a01ab5979ed78b
Quelldatensatz
uspto-grants-1978_03
Patentnummer
US04077795

Notizen zur Reaktion

Wird geladen…