Reaktion #346512

ord-a83ba7cfc42f45ab9be136900302dc0e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat about 20° C.
  2. 2
    Temperaturwarmed to 60° C.
  3. 3
    workup.WAITkept at this temperature for 0.5 hour
  4. 4
    workup.WAITAfter standing overnight at room temperature
  5. 5
    Sonstigethe product is collected
  6. 6
    Waschenwashed with water
  7. 7
    Sonstigeto afford 21 grams, melting point 206° C. to 209° C.

Vorschrift

A sample of 4,5,6,7-tetrahydrobenzo[b]thiophen-4-amine (19.9 grams) is cooled in a flask, and a solution of 12 ml. of 12N hydrochloric acid in 50 ml. of water is slowly added. Subsequently, at about 20° C., a solution of 11.7 grams of potassium cyanate in 80 ml. of water is added in 0.5 hour. The mixture is stirred at room temperature for one hour and then warmed to 60° C. and kept at this temperature for 0.5 hour. After standing overnight at room temperature, the product is collected and washed with water to afford 21 grams, melting point 206° C. to 209° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04036979uspto-grants-1977_07