反応 #461133

ord-1e13144963b84e68964e7c115b7dd202

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度is refluxed for 24 hours
  2. 2
    その他generated is removed by means of an aspirator
  3. 3
    その他The organic and aqueous layers are then separated
  4. 4
    抽出the aqueous layer extracted with ethylacetate
  5. 5
    乾燥The combined organic extracts are dried (magnesium sulfate)
  6. 6
    その他evaporated

実験手順

A mixture of 4-chlorobutyronitrile, (0.05 mol) sodium azide (0.20 mol) and anhydrous aluminum chloride (0.05 mol) in 100 ml of dry tetrahydrofuran is refluxed for 24 hours. After cooling to ambient temperature the reaction is acidified with 75 ml of 15% hydrochloric acid while the hydrazoic acid generated is removed by means of an aspirator. The organic and aqueous layers are then separated and the aqueous layer extracted with ethylacetate. The combined organic extracts are dried (magnesium sulfate) and evaporated to give 5-(3-chloropropyl)tetrazole which is used directly in the next step.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05166210uspto-grants-1992_11