Potassium Carbonate → Ethyl 1-(3-ethoxycarbonylpropylamino)cyclohexanecarboxylate

HRID 975838

Reaktionsgleichung

Reaktionsgleichung von HRID 975838
[NH2:1][C:2]1([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:20][CH2:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24]>>[CH2:26]([O:25][C:23]([CH2:22][CH2:21][CH2:20][NH:1][C:2]1([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1)=[O:24])[CH3:27]

Komponenten

4

Edukt 3

HCID 11430Potassium CarbonateHCID 76300Ethyl 4-bromobutyrateHCID 222863Ethyl 1-aminocyclohexanecarboxylate

Produkt 1

HCID 13282875Ethyl 1-(3-ethoxycarbonylpropylamino)cyclohexanecarboxylate

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

A mixture of ethyl 1-aminocyclohexanecarboxylate (669 g), potassium carbonate (683.1 g) and ethyl 4-bromobutyrate (558 ml) was stirred at 130° C. for 18 hours, then cooled to ambient temperature and poured onto ice-water (3 l). The product was extracted into dichloromethane and the combined extracts were dried over sodium sulphate and the solvent was removed in vacuo to yield ethyl 1-(3-ethoxycarbonylpropylamino)cyclohexanecarboxylate as a brown/orange oil. Yield 943.2 g.

Aufarbeitung

  1. temperaturecooled to ambient temperature
  2. additionpoured onto ice-water (3 l)
  3. extractionThe product was extracted into dichloromethane
  4. dry with materialthe combined extracts were dried over sodium sulphate
  5. customthe solvent was removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-40fb88ba0f324bcc8f0a527c3d225990
Quelldatensatz
uspto-grants-1997_03
Patentnummer
US05610161

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