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Calcium Carbonate → HCID 20446511, Verbindung

HRID 2417753
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2417753
[CH3:1][C:2]1[CH:8]=[C:7]([NH2:9])[C:6]([N+:10]([O-:12])=[O:11])=[CH:5][C:3]=1[NH2:4].C(=O)([O-])[O-].[Ca+2].Br.[Br:19][CH2:20][CH2:21][NH:22]C1C=CC=CC=1>O>[OH2:11].[BrH:19].[CH3:1][C:2]1[CH:8]=[C:7]([NH2:9])[C:6]([N+:10]([O-:12])=[O:11])=[CH:5][C:3]=1[NH:4][CH2:20][CH2:21][NH2:22]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 10112Calcium CarbonateHCID 54879442-Methyl-5-nitrobenzene-1,4-diamineHCID 12606985N-(2-Bromoethyl)aniline--hydrogen bromide (1/1)

Produkt 1

HCID 20446511HCID 20446511, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel3×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A suspension of 0.05 mol (8.35 g) of 2-methyl-4-amino-5-nitroaniline and 0.035 mol (3.5 g) of calcium carbonate in 100 ml of water is heated beforehand on a boiling water-bath, whilst stirring. A solution of 0.07 mol (14.35 g) of β-bromoethylaniline hydrobromide in 20 ml of water is added gradually, whilst stirring. After heating for two hours on the boiling water-bath, the hot reaction medium is filtered. After cooling the filtrate for 24 hours at 0° C., the expected product, which has crystallised in the form of the hydrobromide, is filtered off. The crude product is washed with acetone and then recrystallised from boiling water. After filtration, washing with acetone and drying in vacuo, 2-methyl-4-amino-5-nitro-N-(β-aminoethyl)-aniline hydrobromide monohydrate is obtained.

Aufarbeitung

  1. temperatureis heated beforehand on a boiling water-bath
  2. stirringwhilst stirring
  3. filtrationthe hot reaction medium is filtered
  4. customthe expected product, which has crystallised in the form of the hydrobromide
  5. filtrationis filtered off
  6. washThe crude product is washed with acetone
  7. customrecrystallised
  8. filtrationAfter filtration
  9. washwashing with acetone
  10. customdrying in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-8d058a39995d47acae00c1beac708691
Quelldatensatz
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04470826

Notizen zur Reaktion

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