Reacción #2139246

ord-56549edcbc5647fdae9d8372655f01fa

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    ExtracciónThe base is extracted with methylene chloride
  2. 2
    Secadothe extract dried over potassium carbonate
  3. 3
    Filtraciónfiltered
  4. 4
    Temperaturathe reaction mixture is refluxed for three hours
  5. 5
    FiltraciónThe hot solution is filtered
  6. 6
    Concentraciónconcentrated to a small volume in vacuo, ether
  7. 7
    workup.ADDITIONadded
  8. 8
    Temperaturachilled
  9. 9
    Filtraciónthe solid filtered off

Procedimiento

2-Amino-1-methylimidazoline hydroiodide (26.75 g, 0.117 mole) is converted to its free base form by treatment with 50% sodium hydroxide. The base is extracted with methylene chloride and the extract dried over potassium carbonate and filtered. To this solution is added phenylisothiocyanate (15.81 g, 0.117 mole) and the reaction mixture is refluxed for three hours. The hot solution is filtered, concentrated to a small volume in vacuo, ether added, chilled, and the solid filtered off to give 23.6 g (86.1%) of N-(1-methyl-2-imidazolidinylidene)-N'-phenylthiourea; m.p. 205°-208° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04182865uspto-grants-1980_01