Acetyl chloride → HCID 22668555, Verbindung

HRID 1883729Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1883729
[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][NH:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][CH:7]=1.C(N(CC)CC)C.[C:23](Cl)(=[O:25])[CH3:24]>C(Cl)Cl>[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][N:5]([C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][CH:7]=1)[C:23](=[O:25])[CH3:24]

Komponenten

5

Edukt 3

HCID 6367Acetyl chloride2×HCID 8471Triethylamine2×HCID 22569398HCID 22569398, Verbindung

Produkt 1

HCID 22668555HCID 22668555, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

3.6 g of 4-(2-dimethylamino-ethylamino)-nitrobenzene (according to Gabbay et al., J. Am. Chem. Soc. 91, 5136 (1969)) are dissolved in 50 ml of methylene chloride and 5.0 ml of triethylamine are added. 1.3 ml of acetyl chloride are slowly added dropwise to this mixture at room temperature and the mixture is stirred for 2 hours at room temperature. After this time another 5.0 ml of triethylamine and 1.3 ml of acetylchloride are added and the mixture is refluxed for another 2 hours. The solvent is removed, the residue is taken up in ethyl acetate and the organic phase is extracted twice with water. After drying over MgSO4 the solvent is removed and the residue dried in vacuo.

Aufarbeitung

  1. temperaturethe mixture is refluxed for another 2 hours
  2. customThe solvent is removed
  3. extractionthe organic phase is extracted twice with water
  4. dry with materialAfter drying over MgSO4 the solvent
  5. customis removed
  6. customthe residue dried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-43b54c6d082b4b848d95077a75a21096
Quelldatensatz
uspto-grants-2004_07
Patentnummer
US06762180B1

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