Reaktion #815753

ord-788fc722460140e0aa3f50b30f09ec42

Lösungsmittel

Reaktionsbedingungen

Temperatur
-78°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction was warmed to 0° C. for 4 h
  2. 2
    Temperaturcooled to -78° C
  3. 3
    SonstigeThe reaction was quenched by the addition of 5 ml methanol
  4. 4
    Sonstigethe solvent was evaporated
  5. 5
    SonstigeThe 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).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05049564uspto-grants-1991_09