Reaction #722520

ord-74e0418616e94647b676dce864778aaf

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturethe stirred mixture was heated
  2. 2
    Temperatureunder reflux for 10 minutes
  3. 3
    FiltrationThe resulting solid was collected by filtration
  4. 4
    Washwashed with ethanol (50 ml)
  5. 5
    Otherdried in vacuo at 60° C. for 4 hours

Procedure

A solution of imidazolidine-2-thione (4.5 g) in acetone (750 ml ) was added to a solution of 2-bromo-1-[1-(3,4-dichlorophenyl)cyclobutyl]ethanone (15 g) in acetone (125 ml), then the stirred mixture was heated under reflux for 10 minutes, and allowed to cool to ambient temperature. The resulting solid was collected by filtration, washed with ethanol (50 ml) and dried in vacuo at 60° C. for 4 hours to give 1-[1-(3,4-dichlorophenyl)cyclobutyl]-2-(2-imidazolin-2-ylthio)ethanone hydrobromide as a white solid (16.3 g), m.p. 156-158° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06187802B1uspto-grants-2001_02