反应详情

To a stirred solution of 3.7 parts of (phenylmethyl) carbonochloridate and 2.1 parts of N,N-diethylethanamine in 75 parts of trichloromethane is added dropwise a solution of 4.6 parts of methyl 4-(phenylamino)-4-piperidinecarboxylate in 30 parts of trichloromethane (exothermic reaction: cooling with ice-water is necessary to keep the temperature below 25° C). Upon completion, stirring is continued for 5 hours at room temperature. The reaction mixture is washed twice with water, dried filtered and evaporated. The residue is purified by column-chromatography over silica gel using trichloromethane as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 2-propanol, yielding 4.2 parts of O4 -methyl O1 -(phenylmethyl) 4-(phenylamino)-1,4-piperidinedicarboxylate; mp. 105.8° C.

1. customexothermic reaction
2. customthe temperature below 25° C
3. washThe reaction mixture is washed twice with water
4. customdried
5. filtrationfiltered
6. customevaporated
7. customThe residue is purified by column-chromatography over silica gel
8. customThe pure fractions are collected
9. customthe eluent is evaporated
10. customThe residue is crystallized from 2-propanol