Reaktion #4309

ord-53878bc16b5f4166be999b2b304deda7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent is removed by rotary evaporation (vacuum pump)
  2. 2
    Sonstigethe residue is partitioned between water (
  3. 3
    workup.ADDITIONpH adjusted to 7 by the addition of dilute hydrochloric acid) and chloroform
  4. 4
    SonstigeThe chloroform is removed
  5. 5
    SonstigeThe salt is then recrystallized from methanol-diethyl ether

Vorschrift

A solution of N-[2-[(4-chlorophenyl)sulfonyl]ethyl]-1-methylethanamine hydrochloride and sodium hydroxide in 500 ml of dimethyl sulfoxide is heated at 95° C. for 2 hrs with stirring. The solvent is removed by rotary evaporation (vacuum pump) and the residue is partitioned between water (pH adjusted to 7 by the addition of dilute hydrochloric acid) and chloroform. The chloroform is removed and the residue is converted to the hydrochloride salt with ethereal hydrogen chloride. The salt is then recrystallized from methanol-diethyl ether to give crystalline title compound.

Quelle

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