反应详情

A mixture of 25 parts of N2 -(2-ethoxyethyl)-2,3-pyridinediamine, 43 parts of ethyl 4-isothiocyanato-1-piperidinecarboxylate and 450 parts of tetrahydrofuran was stirred overnight at reflux temperature. The reaction mixture was evaporated and the residue was taken up in trichloromethane. The organic layer was washed twice with water, dried, filtered and evaporated. The residue was crystallized from a mixture of acetonitrile and 2,2'-oxybispropane. The product was filtered off and dried, yielding 35 parts (73.7%) of ethyl 4-[[[[2-[(2-ethoxyethyl)amino]-3-pyridinyl]amino]thioxomethyl]amino]-1-piperidinecarboxylate as a residue (interm. 10).

1. temperatureat reflux temperature
2. customThe reaction mixture was evaporated
3. washThe organic layer was washed twice with water
4. customdried
5. filtrationfiltered
6. customevaporated
7. customThe residue was crystallized from a mixture of acetonitrile and 2,2'-oxybispropane
8. filtrationThe product was filtered off
9. customdried