Reaktion #55283

ord-95b0801eb1af422b91d722b853fc31cf

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA heavy oil formed
  2. 2
    workup.ADDITIONafter the addition
  3. 3
    SonstigeThe oil crystallized
  4. 4
    workup.STIRRINGafter stirring at room temperature for 15 min
  5. 5
    FiltrationThe precipitate was collected by filtration

Vorschrift

An emulsion of 14 g of 3-carbethoxythiomorpholine in 50 ml of n-hexane was added dropwise to a solution of 14 g of 4-chloro-2-fluorophenylisocyanate in 60 ml of anhydrous ether at 15° to 28° C. with stirring. A heavy oil formed after the addition. The oil crystallized after stirring at room temperature for 15 min. The precipitate was collected by filtration to give 24.3 g of 3-carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine, m.p. 111.5°-112.5° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04220465uspto-grants-1980_09