Reaktion #350756

ord-559caf03a51b4fea8830c032fcafea87

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooling
  2. 2
    Sonstigewas returned to room temperature
  3. 3
    workup.STIRRINGstirred overnight
  4. 4
    ExtraktionThe mixture was extracted with chloroform three times
  5. 5
    ExtraktionThe combined extract
  6. 6
    Waschenwas washed with a saturated aqueous sodium chloride solution
  7. 7
    Trocknendried over magnesium sulfate
  8. 8
    workup.DISTILLATIONThe solvent was distilled off
  9. 9
    Sonstigethe resulting crystals were recrystallized from dimethylformamide

Vorschrift

In 150 ml of chloroform-ethanol was suspended 3.40 g of 2-(3-methoxy-4-methylthiophenyl)-4-(3,4-dihydrocarbostyril-6-yl)thiazole. Thereto was added, in small portions, 1.97 g of methachloroperbenzoic acid (80%) under ice-cooling. The mixture was stirred for 1 hour. Then, the mixture was returned to room temperature and stirred overnight. Thereto was added an aqueous sodium carbonate solution. The mixture was extracted with chloroform three times. The combined extract was washed with a saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was distilled off and the resulting crystals were recrystallized from dimethylformamide to obtain 0.50 g of 2-(3-methoxy-4-methylsulfinylphenyl)-4-(3,4-dihydrocarbostyril-6-yl)thiazole as light yellow acicular crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05643932uspto-grants-1997_07