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Potassium Carbonate → HCID 20079712, Verbindung

HRID 1654159
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1654159
[CH3:1][NH:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][CH:6]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][CH:20]([CH3:23])[CH2:21][Cl:22]>CN(C)C=O>[Cl:11][C:8]1[CH:9]=[CH:10][C:5]([CH2:4][CH2:3][N:2]([CH2:19][CH:20]([CH3:23])[CH2:21][Cl:22])[CH3:1])=[CH:6][CH:7]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 955661-Bromo-3-chloro-2-methylpropaneHCID 135897732-(4-Chlorophenyl)-N-methylethan-1-amine

Produkt 1

HCID 20079712HCID 20079712, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

16.9 g (0.1 mol) of N-methyl-2-(4-chlorophenyl)ethylamine were dissolved in 30 ml of dimethylformamide and treated with 20.7 g (0.3 mol) of anhydrous potassium carbonate. The mixture was stirred at 5° and treated with 12.6 ml (0.11 mol) of 1-bromo-2-methyl-3-chloropropane, whereupon the mixture was stirred at 30° for a further 4 hours, the solvent was evaporated at 30° under reduced pressure and the residue was treated with water. The separated oil was extracted three times with ether. The organic extracts were dried over magnesium sulphate and evaporated under reduced pressure. The residual oil was distilled at 135°-140°/260 Pa, whereby there was obtained rac-4-chloro-N-(3-chloro-2-methylpropyl)-N-methylphenethylamine as a colourless oil which was used directly in the next step. MS: 260 (M)+.

Aufarbeitung

  1. stirringwas stirred at 30° for a further 4 hours
  2. customthe solvent was evaporated at 30° under reduced pressure
  3. additionthe residue was treated with water
  4. extractionThe separated oil was extracted three times with ether
  5. dry with materialThe organic extracts were dried over magnesium sulphate
  6. customevaporated under reduced pressure
  7. distillationThe residual oil was distilled at 135°-140°/260 Pa

Quellen und Nachweise

ORD-Eintrag
ord-3ccab5c8439e49d68700f4398631b8a7
Quelldatensatz
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05405866

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