Reaction #4348

ord-10a5e567c3634c778989865c564fb6c3

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturethe mixture was heated to temperature of from 150° to 160° C.
  2. 2
    Temperaturemaintained
  3. 3
    Otherthe crystals thus deposited were collected
  4. 4
    workup.DISSOLUTIONThe crystals were dissolved in an aqueous solution of sodium hydroxide
  5. 5
    Filtrationthe solution was filtered
  6. 6
    Filtrationthe crystals thus deposited were collected by filtration

Procedure

23.1 g of 3-methoxy-6-methylaniline and 16.4 g of sulfamic acid were put into a 100 ml egg-plant type flask and the mixture was heated to temperature of from 150° to 160° C. and maintained thereat for 2 hours. Acetonitrile was added to the reaction mixture and the crystals thus deposited were collected. The crystals were dissolved in an aqueous solution of sodium hydroxide, the solution was filtered and acidified with hydrochloric acid, and the crystals thus deposited were collected by filtration.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04725531uspto-grants-1988_02