反応 #2275124

反応方程式

ethyl 3-[2-(2-aminoethoxy)-4-cyanophenyl]propionate hydrochloride

triethylamine

ethyl 1-(2-chloropyridine-4-yl)-4-piperidinecarboxylate

hydrochloric acid

→

title compound

ethyl 3-[4-cyano-2-(2-((1-(2-chloropyrimidine-4-yl)piperidine-4-carbonyl)amino)ethoxy)phenyl]propionate

溶媒

DMF

ethyl acetate

dioxane

反応条件

後処理

1. 1
   その他The solvent was evaporated
2. 2
   その他the obtained crude product
3. 3
   workup.STIRRINGwere stirred overnight
4. 4
   その他was purified by the silica gel column chromatography

実験手順

700 mg (2.60 mmol) of ethyl 1-(2-chloropyridine-4-yl)-4-piperidinecarboxylate was stirred in 5 ml of dioxane. 5 ml of 2 N hydrochloric acid was added to the obtained mixture, and they were stirred at 95° C. for 4 hours. The solvent was evaporated, and the obtained crude product was dissolved in 10 ml of DMF. 600 mg (2.16 mmol) of ethyl 3-[2-(2-aminoethoxy)-4-cyanophenyl]propionate hydrochloride, 548 mg (3.24 mmol) of 2-chloro-1,3-dimethylimidazonium chloride and 0.9 ml (6.48 mmol) of triethylamine were added to the obtained solution, and they were stirred overnight. After the treatment with ethyl acetate as the extraction solvent in an ordinary manner, the obtained crude product was purified by the silica gel column chromatography to obtain the title compound.

出典