반응 #678084

ord-b3fa5b78f1d24e5a9611d5eead843c73

반응 조건

온도
-78°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITfor 10 minutes
  2. 2
    workup.STIRRINGfurther stirred for 30 minutes
  3. 3
    온도After a temperature was raised to room temperature
  4. 4
    workup.STIRRINGthe reactant was stirred for 1 hour
  5. 5
    기타the reaction was terminated
  6. 6
    온도by cool water
  7. 7
    추출the resultant was extracted with ethylacetate
  8. 8
    workup.DISTILLATIONfollowed by distillation under reduced pressure and column chromatography

실험 절차

After 1.0 g of 1,5-bis-(2-ethylhexyloxy)-2,6-dibromonaphthalene (1.8 mmol) was dissolved in 20 mL of tetrahydrofuran (THF), a temperature was raised to −78° C., and n-butyl lithium was slowly added thereto for 30 minutes. The mixture was stirred at −78° C. for 2 hours, and then 0.46 g of DMF (6.3 mmol) was slowly added thereto for 10 minutes and further stirred for 30 minutes. After a temperature was raised to room temperature and the reactant was stirred for 1 hour, the reaction was terminated by cool water, and the resultant was extracted with ethylacetate, followed by distillation under reduced pressure and column chromatography, thereby obtaining 1.1 g of the title compound (45.0%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09236573B2uspto-grants-2016_01