反应详情

A mixture of 51 parts of methyl 4-(4-chloro-2nitrophenylamino)-3-methyl-1-piperidinecarboxylate, 270 parts of tetrahydrofuran and 96 parts of methanol is hydrogenated at normal pressure and at normal temperature with 15 parts of raney-nickel catalyst. After the calculated amount of hydrogen is taken up (6 hours), the catalyst is filtered off and the filtrate is evaporated. The oily residue is triturated in warm 2,2'-oxybispropane. After cooling, the product is filtered off, pulverized in a mortar and triturated again in 2,2'-oxybispropane. The product is filtered off and dried, yielding methyl 4-(2-amino-4-chlorophenylamino)-3-methyl-1-piperidinecarboxylate.

1. custom(6 hours)
2. filtrationthe catalyst is filtered off
3. customthe filtrate is evaporated
4. customThe oily residue is triturated in warm 2,2'-oxybispropane
5. temperatureAfter cooling
6. filtrationthe product is filtered off
7. customtriturated again in 2,2'-oxybispropane
8. filtrationThe product is filtered off
9. customdried