反应详情

A mixture of 10 parts of ethyl 4-[(2,6-dimethylphenyl)amino]-1-piperidinecarboxylate and 135 parts of hydrobromic acid solution 48% is stirred at a temperature between 80° and 110° C. until the evolution of gaseous carbon dioxide is ceased (about one hour). The red-coloured reaction mixture is evaporated in vacuo. The residue is taken up in 56 parts of methylbenzene and the latter is evaporated again. Then evaporation is repeated in a mixture of 24 parts of 2-propanone and 40 parts of methylbenzene. The resulting semi-solid residue is triturated in 80 parts of hot 2-propanone and on cooling, the solid product is precipitated. It is filtered off, washed successively with small amounts of absolute ethanol and 2-propanone and dried, yielding 13 parts of N-(2,6-dimethylphenyl)-4-piperidinamine dihydrobromide; mp. +300° C.

1. custom(about one hour)
2. customThe red-coloured reaction mixture is evaporated in vacuo
3. customthe latter is evaporated again
4. customThen evaporation
5. additionis repeated in a mixture of 24 parts of 2-propanone and 40 parts of methylbenzene
6. customThe resulting semi-solid residue is triturated in 80 parts of hot 2-propanone
7. temperatureon cooling
8. customthe solid product is precipitated
9. filtrationIt is filtered off
10. washwashed successively with small amounts of absolute ethanol and 2-propanone
11. customdried