Reaktion #69564

Reaktionsgleichung

sodium

1-bromo-3,5-dimethyl adamantane

water

→

product

Ausbeute 159.6%

3,3′,5,5′-tetramethyl-1,1′-biadamantane

Ausbeute 159.6%

Lösungsmittel

n-octane

n-octane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA four-neck 1000 ml flask provided with a thermometer, stirrer
2. 2
   Temperaturreflux tube
3. 3
   workup.ADDITIONwas gradually added dropwise
4. 4
   Sonstigewas kept at 0° C. to 5° C
5. 5
   workup.ADDITIONAfter the end of the dropwise addition, when the temperature
6. 6
   Sonstigethe crude product was separated by filtration
7. 7
   Waschenrinsed with pure water
8. 8
   Sonstigedried
9. 9
   SonstigeFurther, the crude product was recrystallized by hot hexane
10. 10
    SonstigeThe obtained recrystallized product
11. 11
    Sonstigewas dried under reduced pressure

Vorschrift

A four-neck 1000 ml flask provided with a thermometer, stirrer, and reflux tube was charged with metal sodium 14 g (0.6 mol) and n-octane 600 ml and was cooled to an inside temperature of 0° C. While vigorously stirring, 1-bromo-3,5-dimethyl adamantane 73.0 g (0.3 mol) previously dissolved in n-octane 300 ml was gradually added dropwise. While dropping, the inside temperature was kept at 0° C. to 5° C. After the end of the dropwise addition, when the temperature no longer rose, the reaction was continued for 1 hour. After that, the reactant was poured into cold water 1500 ml, then the crude product was separated by filtration, rinsed with pure water, and dried. Further, the crude product was recrystallized by hot hexane. The obtained recrystallized product was dried under reduced pressure to obtain the product 78.2 g.

Quelle