반응 #92776

ord-8b6831b1f2994bb4a02fe57cdc0f99b6

시약

없음

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThe Cu complex (catalytic or stoichiometric amounts) was added
  2. 2
    기타the vial sealed
  3. 3
    기타For the removal of the catalyst complex the reaction mixture
  4. 4
    workup.STIRRINGstirred for 20 min
  5. 5
    기타The complex was removed
  6. 6
    여과by filtering
  7. 7
    농축the filtrate was concentrated
  8. 8
    기타Removal of the solvent
  9. 9
    기타drying of the product in high vacuum

실험 절차

Phenylacetylene (103 mg, 1.0 mmol, 1.0 eq.) and benzyl azide (133 mg, 1.0 mmol, 1.0 eq.) were dissolved in an air-tight lockable vial with a septum in 10 mL dry dichloromethane. The Cu complex (catalytic or stoichiometric amounts) was added, the vial sealed and the reaction stirred at room temperature for 2 days. For the removal of the catalyst complex the reaction mixture was put in 50 mL methanol and stirred for 20 min. The complex was removed by filtering and the filtrate was concentrated. Removal of the solvent and drying of the product in high vacuum resulted in the compound 1-benzyl-4-phenyl-1H-1,2,3-triazole as light yellow solid with 95% yield (245 mg, 0.95 mmol). The identity of the product was proven by NMR-spectroscopy, infrared spectroscopy and high-resolution mass spectroscopy.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09447246B2uspto-grants-2016_09