反应详情

To a stirred and cooled (-10° C.) mixture of 138.6 parts of carbon disulfide, 113.8 parts of N,N'-methanetetraylbis[cyclohexanamine] and 450 parts of tetrahydrofuran were added dropwise 106 parts of methyl 4-amino-3-methyl-1-piperidinecarboxylate at this low temperature. The reaction mixture was allowed to attain room temperature. After stirring for 1 hour at room temperature, the mixture was evaporated and the residue was stirred in 2,2'-oxybispropane. The precipitate was filtered off and the filtrate was evaporated, yielding 141.1 parts (100%) of methyl cis-4-isothiocyanato-3-methyl-1-piperidinecarboxylate as a residue (interm. 28).

1. temperaturecooled
2. customto attain room temperature
3. stirringAfter stirring for 1 hour at room temperature
4. customthe mixture was evaporated
5. stirringthe residue was stirred in 2,2'-oxybispropane
6. filtrationThe precipitate was filtered off
7. customthe filtrate was evaporated