Reaktion #461133

ord-1e13144963b84e68964e7c115b7dd202

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturis refluxed for 24 hours
  2. 2
    Sonstigegenerated is removed by means of an aspirator
  3. 3
    SonstigeThe organic and aqueous layers are then separated
  4. 4
    Extraktionthe aqueous layer extracted with ethylacetate
  5. 5
    TrocknenThe combined organic extracts are dried (magnesium sulfate)
  6. 6
    Sonstigeevaporated

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05166210uspto-grants-1992_11