반응 #1929063

반응 방정식

6-(2-cyan-acetylamino)hexanoic acid

3-dimethylamino-4-methoxybenzaldehyde

piperidine

→

6-[2-cyan-3-(3-dimethylamino-4-methoxy-phenyl)acryloylamino]hexanoic acid

용매

pyridine

반응 조건

후처리

1. 1
   기타After evaporation of the reaction mixture the residue
2. 2
   추출The aqueous phase was extracted with ethyl acetate
3. 3
   세척The collected ethyl acetate phases were washed with NaCl-Solution
4. 4
   기타dried
5. 5
   기타evaporated
6. 6
   기타The residue was chromatographed on SiO2 with ethyl acetate under low pressure
7. 7
   기타The product was crystallized from little ethyl acetate

실험 절차

3.96 g (20 mMol 6-(2-cyan-acetylamino)hexanoic acid was dissolved in 27 ml pyridine. 3.64 g (20 mMol) 3-dimethylamino-4-methoxybenzaldehyde and 0.6 mL piperidine were added to the solution and the reaction mixture was stirred for 20 hours. After evaporation of the reaction mixture the residue was solved in 150 ml ethyl acetate and 150 ml water and the pH was adjusted with pure acetic acid to 4.2. The aqueous phase was extracted with ethyl acetate. The collected ethyl acetate phases were washed with NaCl-Solution, dried and evaporated. The residue was chromatographed on SiO2 with ethyl acetate under low pressure. The product was crystallized from little ethyl acetate.

출처