反应详情

To 1.96 parts of piperidine is added 1.91 parts of potassium iodide and 25 parts deionized water under a nitrogen atmosphere. The mixture is gently warmed and 1.65 parts of potassium hydroxide and 7.51 parts of 2,2-diphenyl-4-bromobutyronitrile are added. The temperature is raised to reflux and maintained thereat for 4.5 hours. After cooling to room temperature, the reaction mixture is extracted three times with 14 part portions of ethyl ether. The ether extracts are combined, and extracted four times with 25 parts by volume portions of a dilute acetic acid solution. The acid extracts are combined, neutralized to about pH 10 with 50% sodium hydroxide solution, and extracted again with ethyl ether. The ether extracts are combined, washed twice with 50 parts by volume portions of a saturated sodium chloride solution, and dried over anhydrous potassium carbonate. The solvent is removed under reduced pressure to afford, as an off-white solid, in 86.1% yield, 2,2-diphenyl-4-piperidinobutyronitrile. This compound melts at 74° - 77° C., and is represented by the following structural formula. ##STR16##

1. temperatureThe mixture is gently warmed
2. temperatureThe temperature is raised
3. temperatureto reflux
4. temperaturemaintained
5. extractionthe reaction mixture is extracted three times with 14 part portions of ethyl ether
6. extractionextracted four times with 25 parts by volume portions of a dilute acetic acid solution
7. extractionextracted again with ethyl ether
8. washwashed twice with 50 parts by volume portions of a saturated sodium chloride solution
9. dry with materialdried over anhydrous potassium carbonate
10. customThe solvent is removed under reduced pressure