Reaction #722528

ord-ce2e6867b5c44f34a3ad635e90430b66

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Otherprepared in a manner similar to
  2. 2
    Temperaturewas heated
  3. 3
    Temperatureunder reflux for 16 hours
  4. 4
    OtherThe solvent was removed in vacuo
  5. 5
    Otherthe residue was triturated with ether (50 ml)
  6. 6
    Filtrationthe resulting solid was collected by filtration
  7. 7
    Washwashed with ether (50 ml)
  8. 8
    Otherdried in vacuo at ambient temperature

Procedure

A suspension of 1-[1-(3,4-dichlorophenyl)cyclobutyl]-2-(3,4,5,6-tetrahydropyrimidin-2-ylthio)ethanone hydrobromide (2.0 g—prepared in a manner similar to that described above) in acetic acid (7 ml) was heated under reflux for 16 hours, then allowed to cool to ambient temperature. The solvent was removed in vacuo, the residue was triturated with ether (50 ml), and the resulting solid was collected by filtration, washed with ether (50 ml), and dried in vacuo at ambient temperature to give 3-[1-(3,4-dichlorophenyl)cyclobutyl]-6,7-dihydro-5H-thiazolo[3,2-a]pyrimidine hydrobromide as a white solid (1.7 g), m.p. 269° C.

Source

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