Reaktion #77247

ord-0e0b7e61abf743bc944f045de8b3f7a3

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationfiltered through a pad of diatomaceous earth with methylene chloride
  2. 2
    Waschenwash
  3. 3
    WaschenThe filtrate is washed with saturated sodium bicarbonate and brine
  4. 4
    Trocknendried over anhydrous magnesium sulfate
  5. 5
    Einengenconcentrated in vacuo to a pale yellow solid, which
  6. 6
    Sonstigeis recrystallized from diethyl ether

Vorschrift

To a mixture of 3-[3-[3-(bromomethyl)-2-thienyl]-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)uracil(1.00 g, 1.99 mmol), methylene chloride and methanol is added silver trifluorormethanesulfonate. The resultant white suspension is stirred overnight at room temperature and filtered through a pad of diatomaceous earth with methylene chloride wash. The filtrate is washed with saturated sodium bicarbonate and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to a pale yellow solid, which is recrystallized from diethyl ether to afford the title compound (0.790 g, 87.7%, mp 131-133° C.) which is identified by NMR spectral analysis.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06706663B2uspto-grants-2004_03