Carbon Dioxide → HCID 23452583, Verbindung

HRID 1278033

Reaktionsgleichung

Reaktionsgleichung von HRID 1278033
C(OC([C:6](=[C:14]1[CH2:18][CH2:17][CH2:16][N:15]1[CH:19]([CH3:21])[CH3:20])[C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1)=O)C.Cl.C(=O)=O>[Pt].[H][H].[OH-].[Na+]>[Cl:13][C:10]1[CH:11]=[CH:12][C:7]([CH2:6][CH:14]2[CH2:18][CH2:17][CH2:16][N:15]2[CH:19]([CH3:21])[CH3:20])=[CH:8][CH:9]=1

Komponenten

6

Edukt 3

HCID 280Carbon DioxideHCID 313Hydrochloric AcidHCID 537817902-(alpha-Ethoxycarbonyl-4-chlorobenzylidene)-1-isopropylpyrrolidine

Produkt 1

HCID 23452583HCID 23452583, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178506450HCID 178506450, VerbindungKatalysatorHCID 14798Sodium HydroxideLösungsmittel

Versuchsvorschrift

Boil 40.6 g of 2-(α-ethoxycarbonyl-4-chlorobenzylidene)-1-isopropylpyrrolidine and 115 ml of conc. hydrochloric acid under reflux until evolution of carbon dioxide ceases. Alkalize the resulting reaction mixture with 250 ml of 6 N sodium hydroxide solution before extracting with 400 ml of diethyl ether, dry the ether phase over sodium sulfate and concentrate it. Dissolve thus-obtained residue in 250 ml of ethanol, and hydrogenate the resulting solution with platinum/hydrogen. Then filter off the catalyst and distil off the solvent before distilling the product under a high vacuum to obtain a yield [21.8 g (70% of theory)] of title compound and having a b.p. of 75° at 7·10-3 mm of Hg.

Aufarbeitung

  1. extractionbefore extracting with 400 ml of diethyl ether
  2. dry with materialdry the ether phase over sodium sulfate
  3. concentrationconcentrate it
  4. dissolutionDissolve
  5. customthus-obtained residue in 250 ml of ethanol
  6. filtrationThen filter off the catalyst
  7. customdistil off the solvent
  8. distillationbefore distilling the product under a high vacuum
  9. customto obtain

Quellen und Nachweise

ORD-Eintrag
ord-d9d447cb75c84b98ac4f0efdbdcbaeb8
Quelldatensatz
uspto-grants-1981_07
Patentnummer
US04279918

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