Dimethylformamide → Ethyl 3-methoxy-4-cyclohexylphenylglyoxylate

HRID 426796Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 426796
[H-].[Na+].[CH3:3]N(C)C=O.[OH:8][C:9]1[CH:10]=[C:11]([C:21](=[O:27])[C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:12]=[CH:13][C:14]=1[CH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1.CI>O>[CH3:3][O:8][C:9]1[CH:10]=[C:11]([C:21](=[O:27])[C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:12]=[CH:13][C:14]=1[CH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1

Komponenten

6

Edukt 4

HCID 6228Dimethylformamide2×HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 20515140HCID 20515140, Verbindung

Produkt 1

HCID 20515180Ethyl 3-methoxy-4-cyclohexylphenylglyoxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a stirred suspension of 0.01 moles of sodium hydride in 25 ml. of dry dimethylformamide which has been cooled to 0° C. is added dropwise a solution of 0.01 moles of ethyl 3-hydroxy-4-cyclohexylphenylglyoxylate in 10 ml. of dimethylformamide. The reaction mixture is stirred for 15 minutes and 0.015 moles of methyliodide is then added dropwise. The mixture is allowed to stir overnight at room temperature. 200 ml. of water is added and the resulting mixture is extracted well with ether. The ether extract is washed with water, dried over sodium sulfate, evaporated to dryness and distilled to obtain ethyl 3-methoxy-4-cyclohexylphenylglyoxylate.

Aufarbeitung

  1. stirringto stir overnight at room temperature
  2. extractionthe resulting mixture is extracted well with ether
  3. extractionThe ether extract
  4. washis washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated to dryness
  7. distillationdistilled

Quellen und Nachweise

ORD-Eintrag
ord-d8f48b053c0745ed9196f35df636eae0
Quelldatensatz
uspto-grants-1979_10
Patentnummer
US04171373

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