Reaction #214901

ord-490f7c74852f44019c3a473b06c7b18d

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturecooled down to 0°-5° C.
  2. 2
    workup.ADDITIONThe addition
  3. 3
    workup.STIRRINGthe reaction mixture was stirred at 5° C. for 30 minutes
  4. 4
    Otherat room temperature
  5. 5
    OtherThe solid that separated
  6. 6
    Otherwas collected
  7. 7
    Otherby decanting and by filtration
  8. 8
    Washwas washed with diethylether

Procedure

To a suspension of 7 g of 1-phenylsemicarbazide in 100 ml of acetonitrile, cooled down to 0°-5° C., were added 7.4 g of β,β-dichloroacryloyl chloride, under stirring. The addition having been completed, the reaction mixture was stirred at 5° C. for 30 minutes and then at room temperature for 1 (one) hour. The solid that separated was collected by decanting and by filtration, then was washed with diethylether, thus obtaining 8 g of 1-(β,β-dichloroacryloyl)-1-phenyl-semicarbazide, in accordance with the elemental analysis and the I.R. and N.M.R. spectra.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04256902uspto-grants-1981_03