反应详情

温度

110 °C

A mixture of 10.4 parts of 4-(phenylamino)-1-(2-phenylethyl)-4-piperidinecarboxylic acid, sodium salt and 75 parts of hexamethylphosphoric triamide is stirred and heated to 110° C. for a while. After cooling to 20° C., 3.63 parts of 3-bromo-1-propene are added dropwise. Upon completion, stirring is continued for 20 hours at room temperature. The reaction mixture is poured onto 150 parts of water and the product is extracted with methylbenzene. The extract is washed with water, dried, filtered and evaporated. The oily residue is purified by column-chromatography over silicagel using a mixture of trichloromethane and 5% of methanol as eluent. The pure fractions are collected and the eluent is evaporated. The oily residue is crystallized from hexane, yielding 2-propenyl 4-(phenylamino)-1-(2-phenylethyl)-4-piperidinecarboxylate; mp. 57.2° C.

1. temperatureAfter cooling to 20° C.
2. stirringUpon completion, stirring
3. extractionthe product is extracted with methylbenzene
4. washThe extract is washed with water
5. customdried
6. filtrationfiltered
7. customevaporated
8. customThe oily residue is purified by column-chromatography over silicagel
9. additiona mixture of trichloromethane and 5% of methanol as eluent
10. customThe pure fractions are collected
11. customthe eluent is evaporated
12. customThe oily residue is crystallized from hexane