Reaktion #452142

ord-41b70cbfcefb4cbab9bd0c62d7050b90

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    WaschenAfter 3 hours the solution was washed with water, 10% aqueous hydrochloric acid solution, brine
  2. 2
    Trocknendried (MgSO4)
  3. 3
    SonstigeEvaporation of the solvent
  4. 4
    workup.WAITleft crude sub-title compound as an oil (8.8 g)

Vorschrift

A solution of diethyl 4-(4-benzofurazanyl)-2-diethoxymethyl-1,4,5,6-tetrahydro-6-hydroxy-6-(trifluoromethyl)-3,5-pyridinedicarboxylate (9.0 g, 17 mmoles), trifluoroacetic anhydride (4.77 ml, 34 mmoles) and pyridine (4.05 ml, 51 mmoles) in dry dichloromethane (100 ml) was stirred at room temperature. After 3 hours the solution was washed with water, 10% aqueous hydrochloric acid solution, brine and dried (MgSO4). Evaporation of the solvent left crude sub-title compound as an oil (8.8 g). Nmr (CDCl3) δ 6.1 (s,H), 5.6(s,H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04607041uspto-grants-1986_08