Реакция #75434

ord-a762b41f09c1473cb4356d6a9dbef19b

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураunder reflux for 16 hours
  2. 2
    ДругоеThe solvent was removed under reduced pressure
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
  4. 4
    ФильтрацияThe solution was filtered
  5. 5
    Сушкаdried with anhydrous sodium sulfate
  6. 6
    ДругоеRemoval of the solvent
  7. 7
    Другоеgave an oil which
  8. 8
    Другоеwas recrystallized from petroleum ether (35-50° C.)

Методика

Sodium bicarbonate (0.42 g, 50 mmol) and dimethylallyl bromide (3.28 g, 22 mmol) were added to a suspension of 2-nitroimidazole (2.26 g, 20 mmol) in dry acetonitrile (10 mL). The mixture was stirred under reflux for 16 hours. The solvent was removed under reduced pressure, and the residue was dissolved in ethyl acetate. The solution was filtered, and dried with anhydrous sodium sulfate. Removal of the solvent gave an oil which was recrystallized from petroleum ether (35-50° C.). Yield 1.83 g, m.p. 48-49° C. 1H NMR (CDCl3) δ7.24 (s, 1H), 7.22 (s, 1H), 5.46 (m, 1H), 5.1 (d, 2H), 1.91 (s, 3H) and 1.90 (s, 3H).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06699458B2uspto-grants-2004_03