反応 #63254

ord-06cd2fb2963b4f3c9f8a55e07e3e2ef8

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他to provide 3.4 g
  2. 2
    その他The solvent was removed under reduced pressure
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
  4. 4
    洗浄The organic solution was washed with water
  5. 5
    その他The organic layer was dried
  6. 6
    その他evaporated

実験手順

Six grams of 2-propylresorcinol and 6.4 g. of 5-bromovaleronitrile were reacted following cedure of Example 2A to provide 3.4 g. of the desired nitrile intermediate. This intermediate was heated to 125° C. overnight with 40 mmoles of tetramethylguanidinium azide in 10 ml. of dimethylformamide. The solvent was removed under reduced pressure and the residue was dissolved in ethyl acetate. The organic solution was washed with water adjusted to pH 6. The organic layer was dried and evaporated to yield the desired subtitle tetrazole intermediate which crystallized after evaporation of the solvent. NMR.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04764521uspto-grants-1988_08