反应详情

A mixture of 10 parts of 2-bromopropane, 9 parts of 4-(methoxymethyl)-N-phenyl-4-piperidinamine, 4.9 parts of N,N-diethylethanamide and 72 parts of N,N-dimethylacetamide is stirred and refluxed for 10.25 hours. After cooling, the formed N,N-diethylethanamine hydrobromide is filtered off and the filtrate is diluted with water. The product is extracted with methylbenzene. The extract is washed thoroughly with water, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (90:10) as eluent. The pure fractions are collected and the eluent is evaporated, yielding 5.7 parts (42.6%) of 4-(methoxymethyl)-1-(1-methylethyl)-N-phenyl-4-piperidinamine as an oily residue.

1. temperaturerefluxed for 10.25 hours
2. temperatureAfter cooling
3. filtrationthe formed N,N-diethylethanamine hydrobromide is filtered off
4. additionthe filtrate is diluted with water
5. extractionThe product is extracted with methylbenzene
6. washThe extract is washed thoroughly with water
7. customdried
8. filtrationfiltered
9. customevaporated
10. customThe residue is purified by column-chromatography over silica gel using
11. additiona mixture of trichloromethane and methanol (90:10) as eluent
12. customThe pure fractions are collected
13. customthe eluent is evaporated