Hydrochloric Acid → 2-(2-Methoxyacetyl)-4-methylcyclohexan-1-one

HRID 621716

Reaktionsgleichung

Reaktionsgleichung von HRID 621716
[H-].[Na+].[CH3:3][CH:4]1[CH2:9][CH2:8][C:7](=[O:10])[CH2:6][CH2:5]1.[C:11]([O:14][CH2:15][CH2:16][O:17]C)(=O)C.Cl>C1C=CC=CC=1.O>[CH3:11][O:14][CH2:15][C:16]([CH:6]1[CH2:5][CH:4]([CH3:3])[CH2:9][CH2:8][C:7]1=[O:10])=[O:17]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 8054Ethylene glycol monomethyl ether acetateHCID 115254-MethylcyclohexanoneHCID 24758Sodium hydride

Produkt 1

HCID 200349082-(2-Methoxyacetyl)-4-methylcyclohexan-1-oneAusbeute 87,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 241BenzeneLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

2.5 g of 60% sodium hydride was suspended in 50 ml of benzene and a mixture of 5.6 g of 4methylcyclohexanone and 5.4 g of methoxyethyl acetate was added dropwise thereto under cooling. After stirring at room temperature for two hours, 20 ml of water was added and the pH value of the reaction mixture was adjusted to 3 with concentrated hydrochloric acid. After removing the benzene phase the aqueous phase was extracted with ether. The benzene solution and the ether solution were combined, washed with water, dried and concentrated to give 7.4 g of crude 2-methoxyacetyl4-methylcyclohexanone. This crude product was subjected to the subsequent step.

Aufarbeitung

  1. additionwas added dropwise
  2. temperatureunder cooling
  3. customAfter removing the benzene phase the aqueous phase
  4. extractionwas extracted with ether
  5. washwashed with water
  6. customdried
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-6d6452be3aa04ad5abfcb8b1671e640f
Quelldatensatz
uspto-grants-1989_04
Patentnummer
US04824952

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