Reaktion #50757

ord-18bf9a7224234c39aa73ac684dbac015

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto precipitate crystals
  2. 2
    FiltrationThe resulting crystals were collected by filtration
  3. 3
    Waschenwashed with 20 ml of isopropyl ether
  4. 4
    Sonstigedried

Vorschrift

In 50 ml of methylene chloride, 10.0 g (0.044 mol) of 2-(5-amino-1,2,4-thiadiazol-3-yl)-2-fluoromethoxyiminoacetic acid hydrate were suspended, followed by the addition of 13.3 g (0.064 mol) of phosphorus pentachloride at -20° C. After stirring for 30 minutes, 100 ml of isopropyl ether were added dropwise to the reaction mixture to precipitate crystals. The resulting crystals were collected by filtration, washed with 20 ml of isopropyl ether and then dried, whereby 9.33 g of a title compound were obtained (yield: 77%, purity: 89.7%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05428173uspto-grants-1995_06