Réaction #64249

ord-804ea5da64ca4972b7c3a4735b112a1e

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreFor the removal of the excess lactone, it
  2. 2
    Filtrationis filtered over a silicic gel acid with ethyl acetate
  3. 3
    AutreAfter collection of the pure fractions, it
  4. 4
    workup.DISTILLATIONis distilled in a vacuum
  5. 5
    Autretriturated with ether
  6. 6
    Filtrationfiltered off with suction

Mode opératoire

4.8 g (0.03 mol) trans-4-nitroxycyclohexylamine are mixed with 5.7 ml 4-butyrolactone and stirred for 3 d at room temperature. For the removal of the excess lactone, it is filtered over a silicic gel acid with ethyl acetate. After collection of the pure fractions, it is distilled in a vacuum, triturated with ether and filtered off with suction. There remain 2.1 g of the title compound of the melting point 58°-60° C., i.e. 28% of theory.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05411989uspto-grants-1995_05