반응 #69564

반응 방정식

sodium

1-bromo-3,5-dimethyl adamantane

water

→

product

수율 159.6%

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

수율 159.6%

용매

n-octane

n-octane

반응 조건

후처리

1. 1
   기타A four-neck 1000 ml flask provided with a thermometer, stirrer
2. 2
   온도reflux tube
3. 3
   workup.ADDITIONwas gradually added dropwise
4. 4
   기타was kept at 0° C. to 5° C
5. 5
   workup.ADDITIONAfter the end of the dropwise addition, when the temperature
6. 6
   기타the crude product was separated by filtration
7. 7
   세척rinsed with pure water
8. 8
   기타dried
9. 9
   기타Further, the crude product was recrystallized by hot hexane
10. 10
    기타The obtained recrystallized product
11. 11
    기타was dried under reduced pressure

실험 절차

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.

출처