Reaction #722521

ord-2265150fff3e4812a6887c87630b65ec

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturewas heated
  2. 2
    Temperatureunder reflux for 18 hours
  3. 3
    OtherThe solvent was removed in vacuo
  4. 4
    Otherthe resulting solid was triturated with ether (50 ml)
  5. 5
    Filtrationcollected by filtration
  6. 6
    Washwashed with ether (50 ml)
  7. 7
    Otherdried in vacuo at 50° C. for 3 hours

Procedure

A stirred suspension of 1-[1-(3,4-dichlorophenyl)cyclobutyl]-2-(2-imidazolin-2-ylthio)ethanone hydrobromide (5 g) in acetic acid (20 ml) was heated under reflux for 18 hours then allowed to cool to ambient temperature. The solvent was removed in vacuo, the residue was allowed to stand at ambient temperature for 24 hours, and the resulting solid was triturated with ether (50 ml), collected by filtration, washed with ether (50 ml) and dried in vacuo at 50° C. for 3 hours to give 3-[1-(3,4-dichlorophenyl)cyclobuty]-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide as a white solid (4.5 g), m.p. 241-244° C.

Source

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