反应 #49749

反应方程式

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

potassium carbonate

cyclopentyl bromide

→

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

收率 98.3%

溶剂

acetonitrile

反应条件

后处理

1. 1
   其他After 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
   萃取extracted with ethyl acetate (100 ml×3 times)
5. 5
   洗涤The organic layer was washed with water
6. 6
   其他dried
7. 7
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

实验过程

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).

来源