Reaktion #2155860

ord-d911287346094a358ac3ef701f001d39

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONwas distilled off
  2. 2
    Filtrationfollowed by filtration

Vorschrift

To a solution of 2-amino-5-bromo benzothiazole (0.23 g, 1.0 mmol) in 1,4-dioxane (8.0 mL) was added ethylisocyanate (3.96 mL, 5.0 mmol) and the resulting solution was heated to 80° C. for 16 h. After the completion of the reaction (TLC monitoring), 1,4-dioxane was distilled off followed by co-distillation with n-hexane (2 times). The residue was then stirred with water at 90° C. for 2 h followed by filtration to obtain the desired product that was further washed with hot water and then dried. The residue was finally washed with ether to obtain the desired product (0.18 g, 60%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08299065B2uspto-grants-2012_10