Reaktion #4314

ord-83cce351f7ce40fbbfb94ec6344ceae4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed in vacuo
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in ether
  3. 3
    ExtraktionThe solution was extracted with three portions of water
  4. 4
    Trocknenwas dried over magnesium sulfate
  5. 5
    workup.ADDITIONwas added until the solution
  6. 6
    SonstigeA white solid precipitated

Vorschrift

A solution of 5.0 g (0.022 mole) of N-[2-(phenylsulfonyl)ethyl]-2-propanamine and 4.30 g (0.025 mole) of 3-(N,N-diethylamino)propylisothiocyanate in 400 ml of acetonitrile was refluxed for 16 hr. The solvent was removed in vacuo and the residue was dissolved in ether. The solution was extracted with three portions of water and was dried over magnesium sulfate. The volume of the ether solution was reduced to 200 ml, and hexane was added until the solution became slightly cloudy. A white solid precipitated to give 6.76 g (76.9%) of white crystalline solid, m.p. 120°-121° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04724235uspto-grants-1988_02