Reaction #722524

ord-b2703ce6696c44799f310dd2f2dbb392

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturethe mixture was heated
  2. 2
    Temperatureunder reflux for 1 hour
  3. 3
    FiltrationThe resulting solid was collected by filtration
  4. 4
    Otherdried in vacuo at ambient temperature

Procedure

A solution of 2-bromo-1-[1-(4-chlorophenyl)cyclobutyl]ethanone (2.9 g) in acetone (25 ml) was added to a solution of 3,4,5,6-tetrahydropyrimidine-2-thiol (1.2 g) in acetone (150 ml), then the mixture was heated under reflux for 1 hour, and allowed to cool to ambient temperature. The resulting solid was collected by filtration and dried in vacuo at ambient temperature to give 1-[1-(4-chlorophenyl)cyclobutyl]-2-(3,4,5,6-tetrahydropyrimidin-2-ylthio)ethanone hydrobromide as a white solid (3.5 g), m.p. 205° C.

Source

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