反応 #565180

ord-b9f2f5421b4d4569a6509ea5288ef395

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture is heated to 40°
  2. 2
    その他the reaction mixture is evaporated
  3. 3
    workup.DISSOLUTIONThe residue is redissolved in water
  4. 4
    抽出The aqueous phase is extracted with methylene chloride (3×30 ml)
  5. 5
    乾燥The organic extracts are dried over potassium carbonate
  6. 6
    その他evaporated

実験手順

A solution of 2.42 g of 5-(p-carboxyphenyl)-5,6,7,8-tetrahydroimidazo[1,5-a]pyridine in 100 ml of ethylene dichloride is treated with 6 ml of concentrated sulfuric acid. The reaction mixture is heated to 40° and 6 ml of hydrazoic acid (2M in ethylene dichloride) is added dropwise. When gas evolution has ceased, the reaction mixture is evaporated. The residue is redissolved in water and adjusted to pH 10. The aqueous phase is extracted with methylene chloride (3×30 ml). The organic extracts are dried over potassium carbonate and evaporated to yield the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04889861uspto-grants-1989_12