Reaktion #84798

ord-e0157a9b9b1041eea07c8cf37f608fa5

Lösungsmittel

Reaktionsbedingungen

Temperatur
-10°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe reaction mixture was quenched with 1 M HCl
  2. 2
    SonstigeThe solid formed
  3. 3
    Sonstigewas collected on a Buchner
  4. 4
    Waschenwashed with H2O
  5. 5
    Sonstigedried under vacuum

Vorschrift

To a solution of 4-(5-ethyl-1,3,4-oxadiazol-2-yl)benzaldehyde (1.6 g, 7.9 mmol) in anhydr DMF (7 mL) was added CHCl3 (2.13 g, 17.8 mmol). After cooling to −10° C., a solution of KOH (0.31 g, 5.5 mmol) in anhydr MeOH (1.5 mL) was added dropwise over 20 min. After stirring at −10° C. for 1 hr, the reaction mixture was quenched with 1 M HCl. The solid formed was collected on a Buchner, washed with H2O and dried under vacuum to give 2,2,2-trichloro-1-(4-(5-ethyl-1,3,4-oxadiazol-2-yl)phenyl)ethanol as a white solid (2.0 g, 80% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434707B2uspto-grants-2016_09