反应详情

A mixture of 18.6 parts of 2,2-diphenyl-4-bromobutyronitrile, 10.0 parts of 4-phenylpiperidine, 8.0 parts of N,N-diisopropylethylamine and 200 parts by volume of 2-methoxyethanol is heated at reflux for 16 hours. The solution is then cooled and stripped in vacuum. The resulting residue is partitioned between dilute sodium hydroxide and ether. Extraction of the ether phase with dilute hydrochloric acid results in the precipitation of an oil. This oil and the aqueous phase of the partitioning are combined, treated with aqueous sodium hydroxide and extracted with 1:1 ether-benzene mixture. The ether-benzene extract is dried over sodium sulfate and stripped in vacuum to give a solid. Crystallization of the solid from a mixture of skelly B and ether provided 2,2-diphenyl-4-(4-phenylpiperidino)butyronitrile, melting at 88° - 89.5° C. and having the following formula ##STR7##

1. temperatureis heated
2. temperatureat reflux for 16 hours
3. temperatureThe solution is then cooled
4. customThe resulting residue is partitioned between dilute sodium hydroxide and ether
5. extractionExtraction of the ether phase with dilute hydrochloric acid
6. customresults in the precipitation of an oil
7. extractionextracted with 1:1 ether-benzene mixture
8. extractionThe ether-benzene extract
9. dry with materialis dried over sodium sulfate
10. customto give a solid
11. customCrystallization of the solid
12. additionfrom a mixture of skelly B and ether