تفاعل #49749

ord-6715bea87faf4002bb023b6804c27c69

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter completion of the reaction, tile solvent
  2. 2
    workup.DISTILLATIONwas distilled off under reduced pressure
  3. 3
    workup.ADDITIONby adding 1N hydrochloric acid (100 ml)
  4. 4
    استخلاصextracted with ethyl acetate (100 ml×3 times)
  5. 5
    غسيلThe organic layer was washed with water
  6. 6
    أخرىdried
  7. 7
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure

الإجراء التجريبي

Then, a solution of the resulting ethyl N-(2-fluoro-4-chloro-5-hydroxyphenyl)carbamate (10.0 g, 42.8 mmol) and potassium carbonate (8.87 g, 64.2 mmol) in acetonitrile (150 ml) was stirred for 1 hour at 80° C. Then, cyclopentyl bromide (9.57 g, 84.2 mmol) was added dropwise thereto, followed by reacting for further 7 hours. After completion of the reaction, tile solvent was distilled off under reduced pressure, and the residue was made acidic by adding 1N hydrochloric acid (100 ml) and extracted with ethyl acetate (100 ml×3 times). The organic layer was washed with water, dried, and the solvent was distilled off under reduced pressure to obtain ethyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate (12.7 g, 98% yield).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05424277uspto-grants-1995_06