Reaktion #160781

ord-36e5daa9d98c4f339d3cd7bf710c73a9

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeUpon removal of volatiles in vacuo, ethyl acetate
  2. 2
    workup.ADDITIONwas added
  3. 3
    Waschenthe solution was washed with Na2CO3(sat.), with NaCl(sat.)
  4. 4
    Trocknenwas dried over MgSO4
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated

Vorschrift

A solution of 2,6-difluorobenzothioamide (1.0 eq) and ethylbromopyruvate (1.0 eq.) in ethanol (1.0 M) was heated in the microwave at 130° C. for 30 minutes. Upon removal of volatiles in vacuo, ethyl acetate was added and the solution was washed with Na2CO3(sat.), with NaCl(sat.), was dried over MgSO4, filtered and concentrated yielding ethyl 2-(2,6-difluorophenyl)thiazole-4-carboxylate (84%). LCMS (m/z): 270.1 (MH+); LC Rt=3.79 min.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829193B2uspto-grants-2014_09