Reaktion #815753
ord-788fc722460140e0aa3f50b30f09ec42
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
-78°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturThe reaction was warmed to 0° C. for 4 h
- 2Temperaturcooled to -78° C
- 3SonstigeThe reaction was quenched by the addition of 5 ml methanol
- 4Sonstigethe solvent was evaporated
- 5SonstigeThe resulting solid was recrystallized from ethanol and ether
Vorschrift
The product from Example 9 (0.490 g) was dissolved in 25 ml methylene chloride and cooled to -78° C. To the reaction was added 0.69 ml BBr3. The reaction was warmed to 0° C. for 4 h and then cooled to -78° C. The reaction was quenched by the addition of 5 ml methanol and the solvent was evaporated. The resulting solid was recrystallized from ethanol and ether to yield 0.470 g white solid, mp: 187-9° C. NMR (d6DMSO) δ 0.88 (t, 3H), 1.65 (m, 2H), 2.60-4.10 (m, 10H), 6.65 (d, 1H), 6.70 (d, 1H), 7.05 (t, 1H).