Reaktion #480872

ord-6b47c1e01b2447308fc8e10bfe12c007

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with diethyl ether (4×25 ml)
  2. 2
    WaschenThe combined organics were washed with saturated sodium bicarbonate solution (3×20 ml) and brine (20 ml)
  3. 3
    Trocknendried (MgSO4)
  4. 4
    Filtrationfiltered
  5. 5
    Sonstigeevaporated under reduced pressure

Vorschrift

4-Iodomethyltetrahydropyran-4-carboxylic acid methyl ester (3.05 g) was dissolved in N,N-dimethylformamide (20 ml) at room temperature and potassium thioacetate (1.47 g) added. The mixture was stirred for 18 hours then diluted with water (50 ml) and extracted with diethyl ether (4×25 ml). The combined organics were washed with saturated sodium bicarbonate solution (3×20 ml) and brine (20 ml), then dried (MgSO4), filtered and evaporated under reduced pressure to give the title compound as a yellow solid (2.42 g, 97%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06809100B2uspto-grants-2004_10