반응 #327952

ord-d3fb472d1f604ee7b3a78794e7b2710c

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was cooled to ambient temperature
  2. 2
    workup.STIRRINGthe vial was stirred unsealed for 10 minutes
  3. 3
    온도heated to 130° C. overnight
  4. 4
    기타The mixture was purified by silica gel chromatography
  5. 5
    세척eluting with a gradient of 5-35% ethyl acetate in hexanes

실험 절차

4-Fluorophenyl acetylene (525 mg, 4.37 mmol) was added to 1,1,1-tributyl-N,N-dimethylstannanamine (1.46 g, 4.37 mmol), and the mixture was stirred in a sealed vial at 50° C. for 2 hours. The mixture was cooled to ambient temperature, and the vial was stirred unsealed for 10 minutes. Benzyl azide (850 μL, 6.80 mmol) was added, and the vial was resealed and heated to 130° C. overnight. The mixture was purified by silica gel chromatography eluting with a gradient of 5-35% ethyl acetate in hexanes to afford the title compound. MS (ESI+) m/z 544.4 (M+H)+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08648069B2uspto-grants-2014_02