反应详情

To a solution of 170 mg of ethyl 2-aminocyclohex-1-enecarboxylate as synthesized in Step 7-1-B in 5 ml of pyridine, 70 mg of phosphorus trichloride was added under cooling with ice, followed by 15 minutes' stirring. Raising the temperature to room temperature, 327 mg of 5-(4-quinoline-2-ylpiperazin-1-yl)hexanoic acid as synthesized in above Step 7-14-C was added to the solution and stirred for 3 hours. Distilling the pyridine off under reduced pressure, the residue was extracted with ethyl acetate and washed with water. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was concentrated under reduced pressure. The residue was purified on silica gel column chromatography (ethyl acetate) to provide 182 mg (38%) of ethyl 2-[5-(4-quinolin-2-ylpiperazin-1-yl)hexanoylamino]cyclohex-1-enecarboxylate.

1. temperatureunder cooling with ice
2. additionwas added to the solution
3. stirringstirred for 3 hours
4. distillationDistilling the pyridine off under reduced pressure
5. extractionthe residue was extracted with ethyl acetate
6. washwashed with water
7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
8. concentrationthe solvent was concentrated under reduced pressure
9. customThe residue was purified on silica gel column chromatography (ethyl acetate)