反応 #351242

ord-4b9267ecfe9c4af8b99dc2952925e96e

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The resulting solution was heated
  2. 2
    温度to reflux for 24 hours
  3. 3
    温度The solution was then cooled
  4. 4
    濃縮concentrated in vacuo
  5. 5
    workup.DISSOLUTIONThe residue was redissolved in ether
  6. 6
    濃縮This was then concentrated in vacuo

実験手順

To a suspension of the material from step (a) (5.1 g, 0.016 mol) in dioxane (150 mL) at room temperature was added tri-n-butyltin azide (9.36 g, 0.016 mol) under N2 with stirring. The resulting solution was heated to reflux for 24 hours. The solution was then cooled and concentrated in vacuo. The residue was redissolved in ether and HCl gas was then passed through the solution for 30 minutes. This was then concentrated in vacuo to give β-(1H-tetrazol-5-yl)-N-(2,4,6-trimethoxyphenyl)benzene propanamide as a white solid (2.1 g) which was used without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05646170uspto-grants-1997_07