Sulfuric Acid → 6,7-Dihydro-2-methyl-4(5H) benzofuranone

HRID 1252794

Reaktionsgleichung

Reaktionsgleichung von HRID 1252794
OS(O)(=O)=O.O[C:7]1[CH2:12][CH2:11][CH2:10][C:9](=[O:13])[C:8]=1[CH2:14][C:15](=[O:17])[CH3:16]>C(Cl)Cl>[CH3:16][C:15]1[O:17][C:7]2[CH2:12][CH2:11][CH2:10][C:9](=[O:13])[C:8]=2[CH:14]=1

Komponenten

4

Edukt 2

HCID 1118Sulfuric AcidHCID 74817023-Hydroxy-2-(2-oxopropyl)-2-cyclohexen-1-one

Produkt 1

HCID 64216646,7-Dihydro-2-methyl-4(5H) benzofuranone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of conc. H2SO4 (300 ml) cooled in an ice-bath was added a solution of 3-hydroxy-2(2-oxopropyl)-2-cyclohexene-1-one (190 g in 300 ml CH2Cl2). Upon completion of addition, the mixture was stirred at ambient temperature for about 1 hour. The mixture was then slowly poured into 3 l ice water, and then about 1 l of CH2Cl2 was added. The layers are separated and the aqueous layer extracted thrice with CH2Cl2 and the combined CH2Cl2 layers again extracted thrice with water. The CH2Cl2 layer washed thrice with dilute aqueous NaHCO3, then once with water and dried (MgSO4). Concentration in vacuo afford an orange oil.

Aufarbeitung

  1. additionUpon completion of addition
  2. customThe layers are separated
  3. extractionthe aqueous layer extracted thrice with CH2Cl2
  4. washThe CH2Cl2 layer washed thrice with dilute aqueous NaHCO3
  5. dry with materialonce with water and dried (MgSO4)
  6. concentrationConcentration in vacuo
  7. customafford an orange oil

Quellen und Nachweise

ORD-Eintrag
ord-27938cde0583418c82206b978208bd88
Quelldatensatz
uspto-grants-1988_05
Patentnummer
US04745222

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