Reaktion #676463

ord-0247623088074d76875e4ab95f35e7c3

Lösungsmittel

Reaktionsbedingungen

Temperatur
140°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe reaction mixture was cooled to room temperature
  2. 2
    Extraktionextracted with tert-butyl methyl ether 3 times
  3. 3
    WaschenThe combined organic layer was washed with water
  4. 4
    TrocknenThe mixture was dried over magnesium sulfate
  5. 5
    Einengenconcentrated under reduced pressure

Vorschrift

A mixture of 1.11 g of 2-fluoro-4-(trifluoromethyl)benzaldehyde, 739 mg of methyl thioglycolate, 1.3 g of potassium carbonate and 20 ml of DMF was stirred at 140° C. for hours, and then the reaction mixture was cooled to room temperature. To the reaction mixture was added water, and then extracted with tert-butyl methyl ether 3 times. The combined organic layer was washed with water, followed by saturated aqueous sodium chloride solution. The mixture was dried over magnesium sulfate, and then concentrated under reduced pressure to obtain 848 mg of methyl 6-(trifluoromethyl)benzo[b]thiophene-2-carboxylate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09232792B2uspto-grants-2016_01