반응 #327953

ord-db41fc845266421baee24a8370fff188

반응 조건

온도
70°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 5-45% ethyl acetate in hexanes

실험 절차

2-Ethynyl toluene (456 μL, 3.62 mmol) was added to 1,1,1-tributyl-N,N-dimethylstannanamine (1.21 g, 3.62 mmol), and the mixture was stirred in a sealed vial at 70° C. for 3 hours. The mixture was cooled to ambient temperature, and the vial was stirred unsealed for 10 minutes. Benzyl azide (678 μL, 5.42 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 5-45% ethyl acetate in hexanes to afford the title compound. MS (ESI+) m/z 539.8 (M+H)+.

출처

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