Dimethylamine → HCID 21552345, Verbindung

HRID 268527

Reaktionsgleichung

Reaktionsgleichung von HRID 268527
[Cl:1][CH2:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]2[N:9]([CH2:22][CH3:23])[C:10]3[C:15]([C:16]=2[CH:17]=1)=[CH:14][C:13]([C:18](=[O:21])[CH2:19]Cl)=[CH:12][CH:11]=3)=[O:4].C([N:26]1[C:38]2C=CC=CC=2C2[C:27]1=CC=CC=2)C.[Cl:39]CC(Cl)=[O:42].[CH3:44][NH:45][CH3:46].[I-].[K+]>CC(=O)CC>[OH2:4].[OH2:42].[ClH:1].[ClH:39].[CH3:27][N:26]([CH2:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]2[N:9]([CH2:22][CH3:23])[C:10]3[C:15]([C:16]=2[CH:17]=1)=[CH:14][C:13]([C:18](=[O:21])[CH2:19][N:45]([CH3:46])[CH3:44])=[CH:12][CH:11]=3)=[O:4])[CH3:38]

Komponenten

7

Edukt 5

HCID 674DimethylamineHCID 4875Potassium IodideHCID 6577Chloroacetyl chlorideHCID 6836N-ethyl carbazoleHCID 21552364HCID 21552364, Verbindung

Produkt 1

HCID 21552345HCID 21552345, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6569Methyl Ethyl KetoneLösungsmittel

Versuchsvorschrift

A mixture of 14.6 g (0.042 mole) of 3,6-bis(chloroacetyl)-N-ethylcarbazole, prepared from N-ethylcarbazole and chloroacetyl chloride, 100 ml of 40% dimethylamine and 7.0 g of potassium iodide in 200 ml of butanone is placed in a Parr bomb and heated at 70°-80°C with stirring for 2 hours. The reaction mixture is cooled and poured into 2.0 l of ice water. The solid which precipitates is filtered off, dissolved in chloroform and dried over magnesium sulfate to give the free base of the desired product which is subsequently converted to the dihydrochloride salt and recrystallized from methanol-acetone to give the desired product.

Aufarbeitung

  1. temperatureheated at 70°-80°C
  2. temperatureThe reaction mixture is cooled
  3. customThe solid which precipitates
  4. filtrationis filtered off
  5. dissolutiondissolved in chloroform
  6. dry with materialdried over magnesium sulfate

Quellen und Nachweise

ORD-Eintrag
ord-94345ce1a48443dcae2a0ec1055a67bc
Quelldatensatz
uspto-grants-1976_03
Patentnummer
US03947593

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