반응 #56440

반응 방정식

2-bromopropane

4-(methoxymethyl)-N-phenyl-4-piperidinamine

N,N-diethylethanamine

→

4-(methoxymethyl)-1-(1-methylethyl)-N-phenyl-4-piperidinamine

수율 42.6%

용매

N,N-dimethylacetamide

반응 조건

후처리

1. 1
   온도refluxed for 10.25 hours
2. 2
   온도After cooling
3. 3
   여과the formed N,N-diethylethanamine hydrobromide is filtered off
4. 4
   workup.ADDITIONthe filtrate is diluted with water
5. 5
   추출The product is extracted with methylbenzene
6. 6
   세척The extract is washed thoroughly with water
7. 7
   기타dried
8. 8
   여과filtered
9. 9
   기타evaporated
10. 10
    기타The residue is purified by column-chromatography over silica gel using
11. 11
    workup.ADDITIONa mixture of trichloromethane and methanol (90:10) as eluent
12. 12
    기타The pure fractions are collected
13. 13
    기타the eluent is evaporated

실험 절차

A mixture of 10 parts of 2-bromopropane, 9 parts of 4-(methoxymethyl)-N-phenyl-4-piperidinamine, 4.9 parts of N,N-diethylethanamine 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.

출처