Reaktion #1116545

ord-b931c63ecf554f069f4279a9ac934fab

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated
  2. 2
    workup.ADDITIONtreated with isopropanol
  3. 3
    TemperaturThe mixture was heated
  4. 4
    workup.DISSOLUTIONto dissolve the product
  5. 5
    workup.ADDITIONwater was added to cloud
  6. 6
    Temperaturthe mixture cooled
  7. 7
    Sonstigeto give crystals

Vorschrift

3-Methyl-1-phenylpyrazolin-5-one (1.74 g, 0.01 mol) was mixed with a methanol solution of 2-ethylthio-3-ethylbenzothiazolium tosylate. Triethylamine (1.01 g, 0.01 mol) was added. The mixture was stirred for 10 minutes, then concentrated and treated with isopropanol. The mixture was heated to dissolve the product, then water was added to cloud, and the mixture cooled to give crystals: 3.22 g (48%), mp 144°-147.5° C., λmax=379 (ε=25,000).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05102781uspto-grants-1992_04