Potassium Carbonate → HCID 53699167, Verbindung

HRID 341049

Reaktionsgleichung

Reaktionsgleichung von HRID 341049
[O:1]=[C:2]1[CH2:7][CH:6]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:5][CH2:4][NH:3]1.I[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.COC1C2C(=C3C(=CC=2)C(OC)=CC=N3)N=CC=1.C(=O)([O-])[O-].[K+].[K+]>CS(C)=O.C(OCC)(=O)C.[Cu]I>[O:1]=[C:2]1[CH2:7][CH:6]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:5][CH2:4][N:3]1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

Komponenten

8

Edukt 4

HCID 11430Potassium CarbonateHCID 11575IodobenzeneHCID 104622984,7-Dimethoxy-1,10-phenanthrolineHCID 18699051Ethyl 2-oxopiperidine-4-carboxylate

Produkt 1

HCID 53699167HCID 53699167, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)KatalysatorHCID 679Dimethyl SulfoxideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Ethyl 2-oxopiperidine-4-carboxylate (0.50 g, 2.9 mmol), iodobenzene (0.77 g, 3.8 mmol, 1.3 equiv), copper(I) iodide (56 mg, 0.29 mmol, 0.1 equiv), 4,7-bis(methoxy)-1,10-phenanthroline (70 mg, 0109 mmol, 0.1 equiv) and potassium carbonate (0.40 g, 3.8 mmol, 1 equiv) were combined in dimethylsulfoxide (10 mL) and placed into a preheated oil bath at 100° C. for 120 hours. The mixture was cooled to ambient temperature, diluted with ethyl acetate (50 mL) and washed with water (2×25 mL) and once with brine (25 mL). The organic extract was dried with sodium sulfate, filtered and concentrated in vacuo, providing the titled compound.

Aufarbeitung

  1. washwashed with water (2×25 mL) and once with brine (25 mL)
  2. extractionThe organic extract
  3. dry with materialwas dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-65f19b2c707d4e4291724a8b8c599f18
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08895580B2

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