Реакция #2171914

ord-4aa777740039406abe6a9dae143ce130

Условия реакции

Температура
0°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.STIRRINGThe reaction mixture was stirred at 0° C. for 2 h
  2. 2
    workup.WAITat room temperature for 1 h
  3. 3
    Температураwith cooling
  4. 4
    ФильтрацияThe precipitate (dark solid) was filtered
  5. 5
    ФильтрацияThe off-white solid was collected by filtration
  6. 6
    ДругоеRecrystallization

Методика

1-Acetamido-3,5-dimethyladamantane (2) (10 g) was added slowly to concentrated sulfuric acid (120 mL) cooled to 0° C. in a salt-ice bath. The solution was stirred at 0° C. for 1 h. Acetonitrile (23 mL) was then added dropwise. The reaction mixture was stirred at 0° C. for 2 h, and then at room temperature for 1 h. The reaction mixture was poured into ice-water. Saturated sodium hydroxide solution was added with cooling. The precipitate (dark solid) was filtered, and discarded. The off-white solid was collected by filtration. Recrystallization afforded 3 as a white solid (6.3 g).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06717012B2uspto-grants-2004_04