Reaktion #669001

ord-09c19c27d4c74db1b901b42351a19f62

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe resulting suspension was sonicated until complete dissolution
  2. 2
    SonstigeThe solvent was removed on a rotary evaporator
  3. 3
    Sonstigeto give a colorless syrup which
  4. 4
    Sonstigewas crystallized from absolute ethanol

Vorschrift

To a solution of compound (XV) (120 mg, 0.495 mmol) in absolute ethanol (5 mL) was added fumaric acid (138 mg, 1.18 mmol). The resulting suspension was sonicated until complete dissolution occurred. The solvent was removed on a rotary evaporator to give a colorless syrup which was crystallized from absolute ethanol to yield 190 mg (88%) of compound (XVI). Mp=142°-143° C. 1H NMR(D2O+TSP): δ 8.71 (s, 1H), 8.64-8.62 (m, 1H), 8.30-8.22 (d, 1H), 7.79-7.72 (m, 1H), 6.60 (s, 3H), 4.58 (s, 1H), 3.90 (s, 1H), 2.90 (s, 3H), 2.80 (s, 1H), 2.46-2.38 (m, 1H), 2.10-1.95 (d, 2H), 1.92-1.62 (m, 5H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05922723uspto-grants-1999_07