反应详情

温度

70 °C

5-Bromopentanoic acid methyl ester (1.22 g) was dissolved in acetonitrile (24.4 ml) and added with potassium carbonate (1.30 g), potassium iodide (0.104 g), and piperidine (0.928 ml) and the whole was stirred at 70° C. for 2.5 hours. The reaction solution was added with water and the whole was subjected to separation/extraction with chloroform. The organic layer was washed with a saturated saline solution and then dried with anhydrous sodium sulfate, followed by concentration under reduced pressure. The residue was again dissolved in 18% hydrochloric acid (20 ml) and the whole was refluxed under heating for 3 hours. The reaction solution was concentrated under reduced pressure. Recrystallization was performed with acetone/acetic acid, thereby obtaining a hydrochloride (1.15 g) of the subject compound as a colorless crystal.

1. extractionthe whole was subjected to separation/extraction with chloroform
2. washThe organic layer was washed with a saturated saline solution
3. dry with materialdried with anhydrous sodium sulfate
4. concentrationfollowed by concentration under reduced pressure
5. dissolutionThe residue was again dissolved in 18% hydrochloric acid (20 ml)
6. temperaturethe whole was refluxed
7. temperatureunder heating for 3 hours
8. concentrationThe reaction solution was concentrated under reduced pressure
9. customRecrystallization