Chloroform → 3-Ethyl-3,5,5-trimethyl-1-(propan-2-yl)piperazin-2-one

HRID 432891

Reaktionsgleichung

Reaktionsgleichung von HRID 432891
[OH-:1].[Na+].[CH:3]([NH:6][CH2:7][C:8]([CH3:11])([NH2:10])[CH3:9])([CH3:5])[CH3:4].[CH:12](Cl)(Cl)Cl.[CH2:16]([C:18]([CH3:20])=O)[CH3:17]>>[CH:3]([N:6]1[CH2:7][C:8]([CH3:11])([CH3:9])[NH:10][C:18]([CH2:16][CH3:17])([CH3:12])[C:20]1=[O:1])([CH3:5])[CH3:4]

Komponenten

5

Edukt 4

HCID 6212ChloroformHCID 6569Methyl Ethyl KetoneHCID 14798Sodium HydroxideHCID 795322-Amino-1,1-dimethylethylisopropylamine

Produkt 1

HCID 125809943-Ethyl-3,5,5-trimethyl-1-(propan-2-yl)piperazin-2-oneAusbeute 33 %

Versuchsvorschrift

40 g (1 mol) of finely ground NaOH are added, with stirring, to a solution of 24.6 g (0.189 mol) of N-1-isopropyl-2-methylpropane-1,2-diamine (prepared in accordance with M. Senkus.: J. Am. Chem. Soc. 68, 10 (1946)) and 25 ml (0.3 mol) of chloroform in 250 ml (2.77 mol) of methyl ethyl ketone at 10° C. The reaction mixture is stirred for 16 hours at room temperature and is then filtered. The filtrate, concentrated by evaporation in a rotary evaporator, is chromatographed over silica gel with hexane/ethyl acetate (3:2). The pure fractions are concentrated by evaporation, giving 13.7 g (33%) of compound (229) in the form of a colourless oil.

Aufarbeitung

  1. filtrationis then filtered
  2. concentrationThe filtrate, concentrated by evaporation in a rotary evaporator
  3. customis chromatographed over silica gel with hexane/ethyl acetate (3:2)
  4. concentrationThe pure fractions are concentrated by evaporation

Quellen und Nachweise

ORD-Eintrag
ord-5cad7f7b6ed0406aa96c01ded5c7288c
Quelldatensatz
uspto-grants-2003_12
Patentnummer
US06664353B2

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