Reaktion #549413

ord-6374fafd84ab42c4a03c9e00a0e91554

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated on the steam bath for 12 hours
  2. 2
    workup.ADDITIONIt is then diluted with 500 ml
  3. 3
    Sonstigethe precipitated yellow solid collected
  4. 4
    Sonstigedried
  5. 5
    SonstigeRecrystallization from 505 aqueous ethanol

Vorschrift

A mixture composed 9.8 g. of 2-(2-chloro-5-thiadiazolyl)-1-methyl-5-nitroimidazole, (Example 16), 11.0 g. of 2,2-diethoxyethylamine, and 250 ml. of dioxane is stirred and heated on the steam bath for 12 hours. It is then diluted with 500 ml. of cold water, cooled, and the precipitated yellow solid collected and dried. Recrystallization from 505 aqueous ethanol gives the pure compound melting at 154°-155° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04065567uspto-grants-1977_12