Hydrochloric Acid → 1-Propanone, 1-(4-methoxy-2,3-dimethylphenyl)-

HRID 370742

Reaktionsgleichung

Reaktionsgleichung von HRID 370742
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[O:9][CH3:10].[C:11](Cl)(=[O:14])[CH2:12][CH3:13].[Cl-].[Al+3].[Cl-].[Cl-].Cl>C(=S)=S>[CH3:8][C:7]1[C:2]([CH3:1])=[C:3]([O:9][CH3:10])[CH:4]=[CH:5][C:6]=1[C:11](=[O:14])[CH2:12][CH3:13]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 62324Propionyl chlorideHCID 762692,3-DimethylanisoleHCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 133066961-Propanone, 1-(4-methoxy-2,3-dimethylphenyl)-Ausbeute 91,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6348Carbon DisulfideLösungsmittel

Versuchsvorschrift

To a stirred solution of 2,3-dimethylanisole (197.0 g) and propionyl chloride (147.0 g) in carbon disulfide (700 ml) is added anhydrous aluminum chloride (232.0 g) at 5°-10° C. over a period of 1.5 hours. Stirring is continued for 2 hours under cooling and additional 3 hours at room temperature. The reaction mixture is poured onto crushed ice--concentrated hydrochloric acid with stirring. The mixture is extracted with chloroform and the chloroform solution is washed successively with water, dilute sodium bicarbonate solution and water and then dried over anhydrous sodium sulfate. After removal of the solvent by evaporation, the residue is distilled at 121°-126° C. (1-2 mmHg) to give the title compound (255.0 g), which is crystallized from n-hexane, m.p. 39°-40° C.

Aufarbeitung

  1. additionThe reaction mixture is poured
  2. customonto crushed ice
  3. extractionThe mixture is extracted with chloroform
  4. washthe chloroform solution is washed successively with water, dilute sodium bicarbonate solution and water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customAfter removal of the solvent
  7. customby evaporation
  8. distillationthe residue is distilled at 121°-126° C. (1-2 mmHg)

Quellen und Nachweise

ORD-Eintrag
ord-e821cf1d067e446f94e7cc973f1392ee
Quelldatensatz
uspto-grants-1985_07
Patentnummer
US04528299

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