반응 #49749

반응 방정식

ethyl N-(2-fluoro-4-chloro-5-hydroxyphenyl)carbamate

potassium carbonate

cyclopentyl bromide

→

ethyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate

수율 98.3%

용매

acetonitrile

반응 조건

후처리

1. 1
   기타After 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
   추출extracted with ethyl acetate (100 ml×3 times)
5. 5
   세척The organic layer was washed with water
6. 6
   기타dried
7. 7
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

실험 절차

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).

출처