Reaktion #80267

ord-e659b523b6ff4b2e9810a224ef5e9207

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTo a 250 ml round-bottomed flask fitted with a reflux condenser, magnetic stirrer, and argon inlet
  2. 2
    workup.ADDITIONAfter addition
  3. 3
    Temperaturthe mixture is heated
  4. 4
    Temperaturto reflux for 2 h
  5. 5
    SonstigeThe product precipitates from the mixture
  6. 6
    Sonstigedried

Vorschrift

To a 250 ml round-bottomed flask fitted with a reflux condenser, magnetic stirrer, and argon inlet are added N,N-bis[2((phenoxycarbonyl)oxy)ethyl]-N-methylamine (25.00 g, 69.6 mmol), acetonitrile (100 ml), and methyl p-toluenesulfonate (12.95 g, 69.6 mmol). After addition is complete, the mixture is heated to reflux for 2 h. The cooled mixture is treated with ether (500 ml). The product precipitates from the mixture and dried to give 5 as a white powder, 31.14 g (81%): mp 117°-118° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05616546uspto-grants-1997_04