Hydrochloric Acid → 3-Methyl-1(3H)-isobenzofuranone

HRID 1061446Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1061446
[C:1]([C:4]1[CH:12]=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7])(=O)[CH3:2].[OH-].[K+].B.[Na].Cl>>[CH3:2][CH:1]1[C:4]2[C:5](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:6](=[O:8])[O:7]1

Komponenten

5

Edukt 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 684742-Acetylbenzoic acidHCID 178418435HCID 178418435, Verbindung

Produkt 1

HCID 189393-Methyl-1(3H)-isobenzofuranoneAusbeute 94,9 %

Versuchsvorschrift

100.96 g of 2-acetylbenzoic acid (3-1) was dissolved in 500 ml of aqueous solution of 41.37 g of potassium hydroxide, to which 20.35 g of sodium boron hydride was added little by little at a room temperature. The resulting mixture was stirred at a room temperature for 2 days, and thereafter, the resulting mixture was adjusted to pH 1 with concentrated hydrochloric acid and extracted with chloroform. The resulting organic layer was dried over anhydrous sodium sulfate, and thereafter, the solvent was distilled off under reduced pressure. The resulting residue was purified by distilling under reduced pressure (117-121° C./3-5 mmHg) to obtain 86.45 g of 3-methylphthalide (3-2).

Aufarbeitung

  1. additionwas added little by little at a room temperature
  2. extractionextracted with chloroform
  3. dry with materialThe resulting organic layer was dried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe resulting residue was purified
  6. distillationby distilling under reduced pressure (117-121° C./3-5 mmHg)

Quellen und Nachweise

ORD-Eintrag
ord-6ea82aaa0dad49ea80f1af01fc666e6a
Quelldatensatz
uspto-grants-2003_02
Patentnummer
US06525066B2

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