Реакция #52103

Уравнение реакции

sodium hydroxide

Acetonitrile

1-Acetamido-3,5-dimethyladamantane

sulfuric acid

→

3

1,7-diacetamido-3,5-dimethyladamantane

Условия реакции

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).

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