Reaktion #669001
ord-09c19c27d4c74db1b901b42351a19f62
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeThe resulting suspension was sonicated until complete dissolution
- 2SonstigeThe solvent was removed on a rotary evaporator
- 3Sonstigeto give a colorless syrup which
- 4Sonstigewas 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).