반응 #425987

ord-476ebcbafa3646deb7240afb08dea68c

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the reaction mixture was refluxed for 5 hours
  2. 2
    기타After volatile materials evaporate
  3. 3
    기타an organic layer was dried
  4. 4
    여과filtered
  5. 5
    기타evaporated
  6. 6
    기타The residual was purified by silica gel column chromatography

실험 절차

In a CCl4 (5 mL) solvent, NBS (N-bromosuccinimide) (10.6 mg, 0.06 mmol) and AIBN (2,2′-azobis(2-methylpropionitrile)) (3.0 mg) were added to a solution of Compound 105 (11.2 mg, 0.03 mmol), and the reaction mixture was refluxed for 5 hours. After volatile materials evaporate, the residual was distributed between ethyl acetate and water, and an organic layer was dried, filtered, and evaporated. The residual was purified by silica gel column chromatography using hexane and ethyl acetate (4:1) to obtain a solid Compound 103 (3.0 mg, 33%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08889881B2uspto-grants-2014_11